CN108503887A - A kind of acicular calcium sulfate and preparation method thereof prepared using desulfurization gypsum powder - Google Patents
A kind of acicular calcium sulfate and preparation method thereof prepared using desulfurization gypsum powder Download PDFInfo
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- CN108503887A CN108503887A CN201810394410.7A CN201810394410A CN108503887A CN 108503887 A CN108503887 A CN 108503887A CN 201810394410 A CN201810394410 A CN 201810394410A CN 108503887 A CN108503887 A CN 108503887A
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- calcium sulfate
- desulfurization gypsum
- gypsum powder
- acicular calcium
- desulfurization
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-containing compounds
-
- 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
- C01F11/466—Conversion of one form of calcium sulfate to another
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/092—Polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/166—Magnesium halide, e.g. magnesium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/016—Additives defined by their aspect ratio
Abstract
The acicular calcium sulfate and preparation method thereof that the invention discloses a kind of to be prepared using desulfurization gypsum powder is obtained by using desulfurated plaster drying ball milling in desulfurization gypsum powder, then by desulfurization gypsum powder and water with 1：4.5~6 proportional arrangement is at slurry, and by adjusting slurry pH, it then mixes and is added in reactor with additive, surfactant, 1~4h of hybrid reaction is carried out under the conditions of 130~150 DEG C, filter cake is dried into 2~5h at 75~120 DEG C after product filtering, it can be prepared by acicular calcium sulfate, the method of the present invention preparation process flow is simple, product draw ratio is high, the mechanical performance of nitrile rubber is obviously improved, using the tail gas desulfurization gypsum of house refuse cracking power generation as raw material, truly realizing turns waste into wealth, and has actual use value and social value.
Description
Technical field
The invention belongs to the regenerative use technology fields of garbage cracking power generation tail gas desulfurization gypsum, and in particular to a kind of utilization
Acicular calcium sulfate and preparation method thereof prepared by desulfurization gypsum powder.
Background technology
Calcic wet desulphurization is widely used in various flue gas desulfurizations due to having the advantages that desulfuration efficiency is high, operating cost is low etc.
Occasion, resulting a large amount of desulfurated plasters, is usually handled, not only waste of resource by way of landfill, and to environment
It adversely affects.And research shows that the content of calcium sulfate is suitable with the natural gypsum in desulfurated plaster, how desulfurated plaster is realized
High-valued regeneration become urgent problem to be solved.Acicular calcium sulfate is due to can conduct with higher middle draw ratio
The additive of basis material achievees the purpose that improve basis material mechanical strength, is widely used in rubber, bituminous industry and friction
Production of material etc..
The advantages that nitrile rubber is due to its high temperature resistant, high intensity, resist chemical and be widely used in making various oil resistant rubbers
Glue product, oil seat gasket, gasket, casing, flexible package, flexible rubber hose, printer's roll, cable glue material etc., in automobile, aviation, stone
Become essential elastic material in the industries such as oil, duplicating.But the disadvantage is that lower temperature resistance is poor, ozone resistance is poor, insulating properties
Can be inferior, elasticity is slightly lower.The shortcomings that in order to make up its poor flexibility, often needs to carry out reinforcement modification to improve the application of rubber
Can, if acicular calcium sulfate can be prepared using desulfurated plaster, and as the reinforcing agent of nitrile rubber, it can not only solve environment
Burden, can also create considerable economic value.
Invention content
In order to solve the deficiencies in the prior art, the purpose of the present invention is to provide it is a kind of it is simple for process, high income, avoid making
It is that pollution generated to environment with organic solvent and can prepare and utilize desulfurated plaster with high average length and draw ratio
Acicular calcium sulfate and preparation method thereof prepared by powder.
In order to realize that above-mentioned technical purpose, the technical solution adopted by the present invention be：
A kind of acicular calcium sulfate prepared using desulfurization gypsum powder, raw material composition and parts by weight are as follows：
35~50 parts of desulfurization gypsum powder；
0.84~11.8 part of additive；
0.5~1.6 part of surfactant；
After the desulfurization gypsum powder is configured to slurry, adds additive and surfactant reacted, by obtained product according to
After sequence is washed, filtered and dried, acicular calcium sulfate is made.
Further, the desulfurated plaster is that the tail gas desulfurization residue of life garbage cracking power generation is dried through 100 DEG C
It is made for 24 hours.
Further, the additive is that at least one of magnesium chloride, citric acid mix.
Further, the surfactant is lauryl sodium sulfate, lauryl sulfosuccinic acid monoester disodium, 12
One kind of sodium alkyl benzene sulfonate or more mixing composition.
A method of preparing acicular calcium sulfate using desulfurization gypsum powder comprising following steps：
Step S1：It is 5~12 μm that desulfurated plaster, which is added in ball mill, and is milled to grain size, obtains desulfurization gypsum powder；
Step S2：By desulfurization gypsum powder and water with 1：4.5~6 proportional arrangement adjusts slurry at slurry, with the dilute sulfuric acid of 10wt%
Expect that pH is 2~4；
Step S3：Step S2 products therefroms are added together with 0.84~11.8 part of additive, 0.5~1.6 part of surfactant
Into reactor, after carrying out 1~4h of hybrid reaction under the conditions of 130~150 DEG C, filtering is washed with water in product, filter cake is in 75
~120 DEG C of 2~5h of drying, you can acicular calcium sulfate is made.
Further, the rotational speed of ball-mill of ball mill is 150r/min in step S1.
Further, the average length of acicular calcium sulfate made from step S3 is 58~76 μm, and draw ratio is 50~68.
Using above-mentioned technical solution, by the way that desulfurated plaster is dried, ball milling, its slurry and magnesium chloride, lemon are enabled
Acicular calcium sulfate is prepared using hydrothermal synthesis method after acid and surfactant blending, compared to anti-solvent recrystallization method, the party
Method has many advantages, such as simple for process, high income, in addition, by the way that desulfurated plaster is carried out ball milling, also reduces the granularity of raw material, makes
The formation for effectively facilitating acicular calcium sulfate crystal form adjusts pH using dilute sulfuric acid, can reach impurity in removal desulfurization gypsum powder
Purpose can provide the calcium sulfate temperature and pressure condition that needle-shaped crystal form is formed, magnesium chloride, citric acid using hydrothermal synthesis method
And the introducing of surfactant effectively slows down the crystallization process of calcium sulfate, achievees the purpose that control calcium sulfate crystal form, finally
Obtained acicular calcium sulfate has high draw ratio, is added in nitrile rubber as reinforcing agent, can significantly improve butyronitrile
The mechanical performances such as tensile strength, the elongation at break of rubber product, have broad application prospects.
Specific implementation mode
A kind of acicular calcium sulfate prepared using desulfurization gypsum powder, raw material composition and parts by weight are as follows：
35~50 parts of desulfurization gypsum powder；
0.84~11.8 part of additive；
0.5~1.6 part of surfactant；
After the desulfurization gypsum powder is configured to slurry, adds additive and surfactant reacted, by obtained product according to
After sequence is washed, filtered and dried, acicular calcium sulfate is made.
Further, the desulfurated plaster is that the tail gas desulfurization residue of life garbage cracking power generation is dried through 100 DEG C
It is made for 24 hours.
Further, the additive is that at least one of magnesium chloride, citric acid mix.
Further, the surfactant is lauryl sodium sulfate, lauryl sulfosuccinic acid monoester disodium, 12
One kind of sodium alkyl benzene sulfonate or more mixing composition.
A method of preparing acicular calcium sulfate using desulfurization gypsum powder comprising following steps：
Step S1：It is 5~12 μm that desulfurated plaster, which is added in ball mill, and is milled to grain size, obtains desulfurization gypsum powder；
Step S2：By desulfurization gypsum powder and water with 1：4.5~6 proportional arrangement adjusts slurry at slurry, with the dilute sulfuric acid of 10wt%
Expect that pH is 2~4；
Step S3：Step S2 products therefroms are added together with 0.84~11.8 part of additive, 0.5~1.6 part of surfactant
Into reactor, after carrying out 1~4h of hybrid reaction under the conditions of 130~150 DEG C, filtering is washed with water in product, filter cake is in 75
~120 DEG C of 2~5h of drying, you can acicular calcium sulfate is made.
Further, the rotational speed of ball-mill of ball mill is 150r/min in step S1.
Further, the average length of acicular calcium sulfate made from step S3 is 58~76 μm, and draw ratio is 50~68.
Embodiment 1
A method of preparing acicular calcium sulfate using desulfurization gypsum powder comprising following steps：
Step S1：Desulfurated plaster is milled to grain size as 6 μm with the rotating speed of 150r/min in the ball mill, obtains desulfurated plaster
Powder；
Step S2：It takes 40 parts of desulfurization gypsum powders to be added to stirring in 240 parts of water and is configured to slurry, then the dilute sulfuric acid tune with 10wt%
It is 3 to save slurry pH；
Step S3：Step S2 products therefroms are added to together with 0.84 part of additive, 0.56 part of surfactant in reactor,
After carrying out hybrid reaction 2h under the conditions of 140 DEG C, filtering is washed with water in product, filter cake dries 3h in 100 DEG C, you can needle is made
Shape calcium sulfate.
Obtained acicular calcium sulfate is detected, the average length for obtaining obtained acicular calcium sulfate is 71 μm,
Draw ratio is 66.
Embodiment 2
A method of preparing acicular calcium sulfate using desulfurization gypsum powder comprising following steps：
Step S1：Desulfurated plaster is milled to grain size as 6 μm with the rotating speed of 150r/min in the ball mill, obtains desulfurated plaster
Powder；
Step S2：It takes 50 parts of desulfurization gypsum powders to be added to stirring in 300 parts of water and is configured to slurry, then the dilute sulfuric acid tune with 10wt%
It is 3 to save slurry pH；
Step S3：Step S2 products therefroms are added to together with 1.84 parts of additives, 0.56 part of surfactant in reactor,
After carrying out hybrid reaction 3h under the conditions of 140 DEG C, filtering is washed with water in product, filter cake dries 3h in 110 DEG C, you can needle is made
Shape calcium sulfate.
Obtained acicular calcium sulfate is detected, the average length for obtaining obtained acicular calcium sulfate is 65 μm,
Draw ratio is 60.
Embodiment 3
A method of preparing acicular calcium sulfate using desulfurization gypsum powder comprising following steps：
Step S1：Desulfurated plaster is milled to grain size as 6 μm with the rotating speed of 150r/min in the ball mill, obtains desulfurated plaster
Powder；
Step S2：It takes 35 parts of desulfurization gypsum powders to be added to stirring in 160 parts of water and is configured to slurry, then the dilute sulfuric acid tune with 10wt%
It is 4 to save slurry pH；
Step S3：Step S2 products therefroms are added to together with 3.9 parts of additives, 0.39 part of surfactant in reactor,
After carrying out hybrid reaction 1h under the conditions of 150 DEG C, filtering is washed with water in product, filter cake dries 4h in 90 DEG C, you can needle is made
Shape calcium sulfate.
Obtained acicular calcium sulfate is detected, the average length for obtaining obtained acicular calcium sulfate is 58 μm,
Draw ratio is 50.
Embodiment 4
A method of preparing acicular calcium sulfate using desulfurization gypsum powder comprising following steps：
Step S1：Desulfurated plaster is milled to grain size as 12 μm with the rotating speed of 150r/min in the ball mill, obtains desulfurated plaster
Powder；
Step S2：It takes 45 parts of desulfurization gypsum powders to be added to stirring in 220 parts of water and is configured to slurry, then the dilute sulfuric acid tune with 10wt%
It is 2 to save slurry pH；
Step S3：Step S2 products therefroms are added to together with 11.8 parts of additives, 1.6 parts of surfactants in reactor,
After carrying out hybrid reaction 2h under the conditions of 140 DEG C, filtering is washed with water in product, filter cake dries 4h in 110 DEG C, you can needle is made
Shape calcium sulfate.
Obtained acicular calcium sulfate is detected, the average length for obtaining obtained acicular calcium sulfate is 60 μm,
Draw ratio is 53.
Embodiment 5
A method of preparing acicular calcium sulfate using desulfurization gypsum powder comprising following steps：
Step S1：Desulfurated plaster is milled to grain size as 5 μm with the rotating speed of 150r/min in the ball mill, obtains desulfurated plaster
Powder；
Step S2：It takes 35 parts of desulfurization gypsum powders to be added to stirring in 210 parts of water and is configured to slurry, then the dilute sulfuric acid tune with 10wt%
It is 3 to save slurry pH；
Step S3：Step S2 products therefroms are added to together with 1.1 parts of additives, 0.5 part of surfactant in reactor,
After carrying out hybrid reaction 2h under the conditions of 140 DEG C, filtering is washed with water in product, filter cake dries 3h in 100 DEG C, you can is made needle-shaped
Calcium sulfate.
Obtained acicular calcium sulfate is detected, the average length for obtaining obtained acicular calcium sulfate is 76 μm,
Draw ratio is 68.
Performance test
The acicular calcium sulfate that above-described embodiment 1~5 is produced is added with the additive amount of 10wt% with thiofide respectively
Enter in nitrile rubber to plasticate, vulcanize, 5 groups of detection samples is made, and performance comparison is carried out with the sample for being not added with acicular calcium sulfate,
Its Shao Er hardness is tested, and measures tensile strength, the elongation at break of rubbery sample according to GB/T 528-2009, it is as a result as follows
Shown in table：
| Project | Shao Er hardness | Tensile strength/MPa | Elongation at break/% |
| Blank group | 43 | 2.0 | 250 |
| Embodiment 1 | 49 | 15.4 | 630 |
| Embodiment 2 | 49 | 14.6 | 600 |
| Embodiment 3 | 47 | 13.0 | 580 |
| Embodiment 4 | 47 | 13.5 | 580 |
| Embodiment 5 | 50 | 16.0 | 650 |
It is added it can be seen from upper table data in embodiment after acicular calcium sulfate product obtained, compared with blank control group, fourth
The Shao Er hardness of nitrile rubber increases, and shows that the addition of the acicular calcium sulfate of the present invention can improve the hardness of nitrile rubber；
In terms of tensile strength and elongation at break, be added to each embodiment product nitrile rubber performance be respectively increased 6 times and 2 times with
On.The performance test results show the acicular calcium sulfate of the invention obtained as the reinforcing agent of nitrile rubber in use, can be substantially
Improve the properties of exterior-coated nitrile rubber article.
The above is the embodiment of the present invention, for the ordinary skill in the art, religion according to the present invention
Lead, without departing from the principles and spirit of the present invention all equivalent changes done according to scope of the present invention patent, repair
Change, replace and modification, should all belong to the covering scope of the present invention.
Claims (7)
1. a kind of acicular calcium sulfate prepared using desulfurization gypsum powder, it is characterised in that：Its raw material forms and parts by weight are as follows：
35~50 parts of desulfurization gypsum powder；
0.84~11.8 part of additive；
0.5~1.6 part of surfactant；
After the desulfurization gypsum powder is configured to slurry, adds additive and surfactant reacted, by obtained product according to
After sequence is washed, filtered and dried, acicular calcium sulfate is made.
2. the acicular calcium sulfate for utilizing desulfurization gypsum powder to prepare according to claim 1, it is characterised in that：The desulfurization stone
Cream is that the tail gas desulfurization residue of life garbage cracking power generation is made for 24 hours through 100 DEG C of drying process.
3. the acicular calcium sulfate for utilizing desulfurization gypsum powder to prepare according to claim 1, it is characterised in that：The additive
It is mixed at least one of magnesium chloride, citric acid.
4. the acicular calcium sulfate for utilizing desulfurization gypsum powder to prepare according to claim 1, it is characterised in that：It lives on the surface
Property agent be that lauryl sodium sulfate, one kind of lauryl sulfosuccinic acid monoester disodium, neopelex or more are mixed
It is combined into.
5. utilizing the preparation method of the acicular calcium sulfate of desulfurization gypsum powder preparation according to claim 1, it is characterised in that：Its
Include the following steps：
Step S1：It is 5~12 μm that desulfurated plaster, which is added in ball mill, and is milled to grain size, obtains desulfurization gypsum powder；
Step S2：By desulfurization gypsum powder and water with 1：4.5~6 proportional arrangement adjusts slurry at slurry, with the dilute sulfuric acid of 10wt%
PH is 2~4；
Step S3：Step S2 products therefroms are added to instead together with 0.1~13 part of additive, 0.1~1.6 part of surfactant
It answers in device, after carrying out 1~4h of hybrid reaction under the conditions of 130~150 DEG C, filtering is washed with water in product, filter cake is in 75~120
DEG C drying 2~5h, you can be made acicular calcium sulfate.
6. utilizing the preparation method of the acicular calcium sulfate of desulfurization gypsum powder preparation according to claim 5, it is characterised in that：Step
The rotational speed of ball-mill of ball mill is 150r/min in rapid S1.
7. utilizing the preparation method of the acicular calcium sulfate of desulfurization gypsum powder preparation according to claim 5, it is characterised in that：Step
The average length of acicular calcium sulfate made from rapid S3 is 58~76 μm, and draw ratio is 50~68.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113428887A (en) * | 2021-08-10 | 2021-09-24 | 桂林理工大学 | Method for preparing alpha high-strength gypsum from industrial byproduct gypsum |
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|---|---|---|---|---|
| CN101550602A (en) * | 2009-05-19 | 2009-10-07 | 武汉科技大学 | CaSO* crystal whisker with desulfurized gypsum as raw material and preparing method |
| CN104496237A (en) * | 2014-12-01 | 2015-04-08 | 路德环境科技股份有限公司 | Method for removing impurities from desulphurization gypsum of power plant |
| CN105568387A (en) * | 2016-02-26 | 2016-05-11 | 烟台大学 | Preparation method of calcium sulfate whiskers |
| CN106801259A (en) * | 2017-01-17 | 2017-06-06 | 辽宁工程技术大学 | A kind of method that mechanical force activating desulfurated plaster prepares calcium sulfate crystal whiskers |
| CN107236993A (en) * | 2017-07-07 | 2017-10-10 | 南开大学 | A kind of method that desulfurated plaster produces calcium sulfate crystal whiskers |
-
2018
- 2018-04-27 CN CN201810394410.7A patent/CN108503887A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550602A (en) * | 2009-05-19 | 2009-10-07 | 武汉科技大学 | CaSO* crystal whisker with desulfurized gypsum as raw material and preparing method |
| CN104496237A (en) * | 2014-12-01 | 2015-04-08 | 路德环境科技股份有限公司 | Method for removing impurities from desulphurization gypsum of power plant |
| CN105568387A (en) * | 2016-02-26 | 2016-05-11 | 烟台大学 | Preparation method of calcium sulfate whiskers |
| CN106801259A (en) * | 2017-01-17 | 2017-06-06 | 辽宁工程技术大学 | A kind of method that mechanical force activating desulfurated plaster prepares calcium sulfate crystal whiskers |
| CN107236993A (en) * | 2017-07-07 | 2017-10-10 | 南开大学 | A kind of method that desulfurated plaster produces calcium sulfate crystal whiskers |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113428887A (en) * | 2021-08-10 | 2021-09-24 | 桂林理工大学 | Method for preparing alpha high-strength gypsum from industrial byproduct gypsum |
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Application publication date: 20180907 |