CN109574060A - A kind of method of desulfurized gypsum removal of impurities decoloration - Google Patents
A kind of method of desulfurized gypsum removal of impurities decoloration Download PDFInfo
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- CN109574060A CN109574060A CN201811557256.7A CN201811557256A CN109574060A CN 109574060 A CN109574060 A CN 109574060A CN 201811557256 A CN201811557256 A CN 201811557256A CN 109574060 A CN109574060 A CN 109574060A
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- desulfurized gypsum
- removal
- washing
- impurities
- crystal
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/468—Purification of calcium sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
- C01P2006/65—Chroma (C*)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
A kind of method that the present invention discloses desulfurized gypsum removal of impurities decoloration.First the processing such as grinding, screening, ultrasound is dried to desulfurized gypsum in this method, it can promote the dispersion of gypsum crystal, be conducive to that there are the removals of the impurity between plane of crystal and crystal, improve washing efficiency, reduce dosage, the discharge for washing waste liquid and the washing times of water, operation is simplified, environmental pollution is reduced.Then, on the basis of ultrasound washing, heating pickling is carried out with sulfuric acid, can promote the release for being wrapped in the foreign pigment of crystals.Pickling after reaction, filters immediately, can prevent impurity during recrystallization, be wrapped among crystal again, to improve the effect of removal of impurities decoloration.Meanwhile with sulphur acid instead of HCl, new impurity will not be introduced.After the method for the invention operates, desulfurized gypsum impurity content is down to 1.27% hereinafter, whiteness increases to 90.69% or more by 30.26% by 2.75%.
Description
Technical field
The present invention relates to inorganic salts technology field more particularly to a kind of methods of desulfurized gypsum removal of impurities decoloration.
Background technique
Desulfurized gypsum, also known as desulfurized gesso of flue gas, FGD gypsum (Flue Gas Desulphurization Gypsum),
It is the by-product of coal fired power plant flue gas desulfurization, main component is calcium sulphate dihydrate (CaSO4·2H2), O separately have 10% or so
The impurity such as free water and a small amount of flying dust, metal oxide.Desulfurized gypsum added value itself is lower, with China industry it is quick
Development, discharges nearly hundred million tons of desulfurized gypsum every year, a large amount of to store up, not only land occupation, waste of resource, but also pollutes environment,
Seriously constrain the sustainable development of China's coal-firing units gas desulfurization.Therefore, the resource utilization of desulfurized gypsum is realized
It is very urgent.
Desulfurized gypsum is (greasy in painting technology in building materials industry (cement, coacervation material, building product etc.), chemical industry
Son and filler material, the filler of plastics industry, production ammonium sulfate fertilizer, improvement saline-alkali soil etc.), process mould and artistic mold etc.
There is huge application potential in field, but more demanding to the whiteness of desulfurized gypsum.Due to impurity such as flying dust, metal oxides
Influence, desulfurized gypsum typically exhibits micro- yellow or canescence, deeper color and limits its extensive resource utilization.
Traditional removal of impurities discoloration method has WATER-WASHING METHOD, washing plus chlorohydric acid pickling method.WATER-WASHING METHOD can only remove gypsum crystal table
Water-solubility impurity between face and crystal is still wrapped around crystals there are many impurity, which not can be removed, therefore remove
The effect of miscellaneous decoloration is limited.In addition, WATER-WASHING METHOD needs a large amount of water every time, and washing repeatedly, causes the waste of water resource repeatedly
And environmental pollution.The characteristics of washing plus chlorohydric acid pickling method are using that can mutually convert between gypsum different crystal, in washing
On the basis of, then with hydrochloric acid, pickling is carried out under heating condition, original gypsum crystal structure is destroyed, it is miscellaneous that removal is wrapped in crystals
The method of matter.Though the method cleans, decolorizing effect is obvious, but still solves the problems, such as the waste and environmental pollution of WATER-WASHING METHOD water resource,
Meanwhile the use of hydrochloric acid, it introduces newly except impurity-chloride ion, it is largely also unfavorable since chloride ion corrosion is higher
In the resource utilization of desulfurized gypsum.
The basic composition and whiteness of desulfurized gypsum raw material used in the present invention are as follows:
CaSO4 | H2O | Impurity | Whiteness |
85.17% | 12.08% | 2.75% | 30.26% |
Summary of the invention
The purpose of the present invention is to overcome the disadvantages of the prior art, provides a kind of efficient, low consumption, environmental protection desulfurized gypsum
Clean the method decolourized.This method can not only remove the impurity in desulfurized gypsum significantly, decolourize to it, improve its whiteness, and
And it can be reduced use and the discharge of wastewater of water, while the new impurity such as do not introduce chlorine root.
What the object of the invention was achieved through the following technical solutions.
A kind of method of desulfurized gypsum removal of impurities decoloration, it including the following steps:
(1) desulfurized gypsum is placed in in 100 DEG C -120 DEG C of baking oven dry 1h-2h, removes free water, it is de- to obtain butt
Sulphur gypsum;
(2) butt desulfurized gypsum is ground, is sieved through 80-100 mesh square hole screen, extracting screen underflow;
(3) ratio that screenings and deionized water are 1:3-5 in mass ratio is added in beaker, then sets beaker
In ultrasonic device, at 30 DEG C -50 DEG C, ultrasound washing 15min-30min is washed while stirring, is filtered, obtain filter cake;
(4) by the dilute sulfuric acid of desulfurized gypsum and 1mol/L after ultrasound washing, add 1mol/L's by every 10g desulfurized gypsum
The ratio of dilute sulfuric acid 150ml-250ml, puts into three-necked flask, is stirred to react 2-3h at 80 DEG C -90 DEG C;
(5) filter reaction solution immediately after reaction, obtain no mother liquor of precipitation of ammonium, mother liquor is transferred to beaker, in 10 DEG C-
At 15 DEG C, 8h-12h is stood, mother liquor is then filtered and obtains filtrate and filter cake, filtrate return step (4) is recycled, and filter cake is placed in
Dry 1h-2h obtains final products in 100 DEG C -120 DEG C of baking oven.
The invention has the benefit that desulfurized gypsum is dried, is ground, is sieved, the processing such as ultrasound, stone can promote
The dispersion of cream crystal is conducive to improve washing efficiency there are the removal of the impurity between plane of crystal and crystal, reduce water
Dosage, wash waste liquid discharge and washing times, simplify operation, reduce environmental pollution.On the basis of ultrasound washing
On, heating pickling is carried out with sulfuric acid, can promote the release for being wrapped in the foreign pigment of crystals.Pickling after reaction, is stood
It filters, can prevent impurity during recrystallization, be wrapped among crystal again, to improve the effect of removal of impurities decoloration.
Meanwhile with sulphur acid instead of HCl, new impurity will not be introduced.After the method for the invention operates, desulfurized gypsum impurity content
1.27% is down to hereinafter, whiteness increases to 90.69% or more by 30.26% by 2.75%.
Specific embodiment
Method provided by the invention is described in detail below with reference to embodiment, but the invention is not limited in any way.
Embodiment 1: concrete operations are as follows
(1) desulfurized gypsum is placed in in 100 DEG C of baking oven dry 2h, free water is removed, obtains butt desulfurized gypsum;
(2) butt desulfurized gypsum is ground, is sieved through 80 mesh square hole screens, extracting screen underflow;
(3) ratio that screenings and deionized water are 1:3 in mass ratio is added in beaker, is then placed the beaker
In ultrasonic device, at 30 DEG C, ultrasound washing 30min is washed while stirring, is filtered, obtain filter cake;
(4) by the dilute sulfuric acid of desulfurized gypsum and 1mol/L after ultrasound washing, add 1mol/L's by every 10g desulfurized gypsum
The ratio of dilute sulfuric acid 150ml, puts into three-necked flask, is stirred to react 2h at 80 DEG C;
(5) it filters reaction solution immediately after reaction, obtains no mother liquor of precipitation of ammonium, mother liquor is transferred to beaker, in 15 DEG C
Under, 12h is stood, mother liquor is then filtered and obtains filtrate and filter cake, filtrate return step (4) is recycled, and filter cake is placed in 100 DEG C
Dry 2h obtains final products in baking oven.
Through detecting, product impurity content is down to 1.27% by 2.75%, and whiteness increases to 90.69% by 30.26%.
Embodiment 2: concrete operations are as follows
(1) desulfurized gypsum is placed in in 110 DEG C of baking oven dry 1.5h, free water is removed, obtains butt desulfurized gypsum;
(2) butt desulfurized gypsum is ground, is sieved through 90 mesh square hole screens, extracting screen underflow;
(3) ratio that screenings and deionized water are 1:4 in mass ratio is added in beaker, is then placed the beaker
In ultrasonic device, at 40 DEG C, ultrasound washing 20min is washed while stirring, is filtered, obtain filter cake;
(4) by the dilute sulfuric acid of desulfurized gypsum and 1mol/L after ultrasound washing, add 1mol/L's by every 10g desulfurized gypsum
The ratio of dilute sulfuric acid 200ml, puts into three-necked flask, is stirred to react 2.5h at 90 DEG C;
(5) it filters reaction solution immediately after reaction, obtains no mother liquor of precipitation of ammonium, mother liquor is transferred to beaker, in 10 DEG C
Under, 8h is stood, mother liquor is then filtered and obtains filtrate and filter cake, filtrate return step (4) is recycled, and filter cake is placed in 120 DEG C of baking
Dry 1h obtains final products in case.
Through detecting, product impurity content is down to 1.19% by 2.75%, and whiteness increases to 91.88% by 30.26%.
Embodiment 3: concrete operations are as follows
(1) desulfurized gypsum is placed in in 120 DEG C of baking oven dry 1h, free water is removed, obtains butt desulfurized gypsum;
(2) butt desulfurized gypsum is ground, is sieved through 100 mesh square hole screens, extracting screen underflow;
(3) ratio that screenings and deionized water are 1:5 in mass ratio is added in beaker, is then placed the beaker
In ultrasonic device, at 50 DEG C, ultrasound washing 15min is washed while stirring, is filtered, obtain filter cake;
(4) by the dilute sulfuric acid of desulfurized gypsum and 1mol/L after ultrasound washing, add 1mol/L's by every 10g desulfurized gypsum
The ratio of dilute sulfuric acid 250ml, puts into three-necked flask, is stirred to react 3h at 85 DEG C;
(5) it filters reaction solution immediately after reaction, obtains no mother liquor of precipitation of ammonium, mother liquor is transferred to beaker, in 13 DEG C
Under, 10h is stood, mother liquor is then filtered and obtains filtrate and filter cake, filtrate return step (4) is recycled, and filter cake is placed in 110 DEG C
Dry 1.5h obtains final products in baking oven.
Through detecting, product impurity content is down to 1.08% by 2.75%, and whiteness increases to 92.17% by 30.26%.
It is all using several made by present specification the foregoing is merely the preferred embodiment of the present invention
It improves or deforms, being applied directly or indirectly in other relevant technical fields, also should be regarded as in patent protection model of the invention
In enclosing.
Claims (6)
1. a kind of method of desulfurized gypsum removal of impurities decoloration, it is characterised in that the following steps are included:
(1) desulfurized gypsum is placed in drying in baking oven, removes free water, obtains butt desulfurized gypsum;
(2) butt desulfurized gypsum is ground, is sieved through square hole screen, extracting screen underflow;
(3) screenings and deionized water are added in beaker, are then placed the beaker in ultrasonic device, while stirring ultrasonic water
Wash, after filter, obtain filter cake;
(4) desulfurized gypsum after ultrasound washing is put into three-necked flask with the dilute sulfuric acid of 1mol/L and is reacted;
(5) it filters reaction solution immediately after reaction, obtains no mother liquor of precipitation of ammonium, mother liquor is transferred to beaker, after being stood under low temperature,
It filters mother liquor and obtains filtrate and filter cake, filtrate return step (4) is recycled, and filter cake, which is placed in baking oven, is dried to obtain final products.
2. the method for desulfurized gypsum removal of impurities decoloration according to claim 1, it is characterised in that dry in the step (1)
Temperature is 100 DEG C -120 DEG C, drying time 1h-2h.
3. the method for desulfurized gypsum removal of impurities decoloration according to claim 1, it is characterised in that square hole in the step (2)
The size of sieve is 80-100 mesh.
4. the method for desulfurized gypsum removal of impurities decoloration according to claim 1, it is characterised in that in the step (3) under sieve
Object and the mass ratio of deionized water are 1:3-5, and the temperature of ultrasound washing is 30 DEG C -50 DEG C, and the time of ultrasound washing is 15min-
30min。
5. the method for desulfurized gypsum removal of impurities decoloration according to claim 1, it is characterised in that feed intake in the step (4)
Ratio is the dilute sulfuric acid 150ml-250ml for adding 1mol/L by every 10g desulfurized gypsum, and reaction condition is to stir instead at 80 DEG C -90 DEG C
Answer 2-3h.
6. the method for desulfurized gypsum removal of impurities decoloration according to claim 1, it is characterised in that stood in the step (5)
Condition is to stand 8h-12h at 10 DEG C -15 DEG C, and drying condition is dry 1h-2h at 100 DEG C -120 DEG C.
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Cited By (4)
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CN111020201A (en) * | 2019-12-27 | 2020-04-17 | 万载志成实业有限公司 | Method for purifying and removing impurities from smelting flue gas desulfurization gypsum |
CN112790322A (en) * | 2021-02-02 | 2021-05-14 | 山东农业大学 | Method for decoloring high-temperature peanut meal for protein |
CN112850773A (en) * | 2021-02-01 | 2021-05-28 | 贵州中亚高科涂料有限公司 | High-efficiency production method of high-purity semi-water desulfurization paste |
CN113149037A (en) * | 2021-05-25 | 2021-07-23 | 天津渤化永利化工股份有限公司 | Method for preparing potassium sulfate by utilizing desulfurized gypsum |
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CN111020201A (en) * | 2019-12-27 | 2020-04-17 | 万载志成实业有限公司 | Method for purifying and removing impurities from smelting flue gas desulfurization gypsum |
CN112850773A (en) * | 2021-02-01 | 2021-05-28 | 贵州中亚高科涂料有限公司 | High-efficiency production method of high-purity semi-water desulfurization paste |
CN112790322A (en) * | 2021-02-02 | 2021-05-14 | 山东农业大学 | Method for decoloring high-temperature peanut meal for protein |
CN113149037A (en) * | 2021-05-25 | 2021-07-23 | 天津渤化永利化工股份有限公司 | Method for preparing potassium sulfate by utilizing desulfurized gypsum |
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Application publication date: 20190405 |