CN113044872A - Preparation method of lanthanum sulfate - Google Patents
Preparation method of lanthanum sulfate Download PDFInfo
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- CN113044872A CN113044872A CN202110400991.2A CN202110400991A CN113044872A CN 113044872 A CN113044872 A CN 113044872A CN 202110400991 A CN202110400991 A CN 202110400991A CN 113044872 A CN113044872 A CN 113044872A
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- Prior art keywords
- lanthanum
- lanthanum sulfate
- water
- sulfate
- sulfuric acid
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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
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- 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
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/282—Sulfates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of lanthanum sulfate, which comprises the steps of carrying out hydration reaction on water, sulfuric acid and lanthanum oxide to obtain lanthanum sulfate, and then filtering, drying and crushing to obtain a finished product of lanthanum sulfate. The whole reaction process is simple, the production cost is low, the economy is considerable, the product quality is stable, meanwhile, the filtrate can be recycled for a plurality of times, no waste water is discharged, and the national environmental protection requirement is met.
Description
Technical Field
The invention relates to synthesis of chemical products, in particular to a preparation method of lanthanum sulfate.
Background
Rare Earth (Rare Earth) is a general name of seventeen metal elements including lanthanide elements, scandium and yttrium in the chemical periodic table. There are 250 kinds of rare-earth ores in nature. The first rare earth discovered was the finnish chemist gardolin (John Gadolin). The first rare earth "element" (yttrytrium earth, Y2O3) was isolated in 1794 from a block of heavy bituminous ore, which was historically known as rare earth because of the small amount of rare earth minerals found in the 18 th century and only a small amount of water-insoluble oxide was produced by chemical means.
China is rich in rare earth resources and is the country with the largest reserves in the world at present. The phosphorous acid rare earth complex has wide application prospect in the aspects of novel luminescent materials, extraction chemistry, displacement reagents, particularly plastic processing stabilizers and the like.
The stabilizer is required to be added during plastic processing, lead phosphite is mostly applied at present, and the stabilizer is a polyvinyl chloride heat stabilizer, has outstanding weather resistance, oxidation resistance and ultraviolet ray shielding capacity, and has excellent thermal stability and electrical insulation. However, lead phosphite has toxic effects on human bodies, can change nervous systems, blood and blood vessels, and has great influence on protein metabolism, cell energy balance and cell genetic systems.
Disclosure of Invention
The invention mainly solves the technical problem of providing a preparation method of lanthanum sulfate, which has low production cost, can greatly reduce the production cost and has stable product quality; meanwhile, the filtrate can be recycled for a plurality of times, no wastewater is discharged, toxic substances such as lead phosphite and the like can be replaced, the national environmental protection requirement is met, and energy is saved.
In order to solve the technical problems, the invention adopts a technical scheme that: the preparation method of lanthanum sulfate comprises the following steps:
step 1, adding a proper amount of water into a reaction kettle, heating and stirring the water, and keeping the water temperature at 20-35 ℃;
step 2, sequentially and continuously dripping sulfuric acid and lanthanum oxide into water, then continuously stirring uniformly, keeping the temperature of the water at 60-65 ℃, and carrying out synthetic reaction on the water, the sulfuric acid and the lanthanum oxide to generate lanthanum sulfate;
step 3, cooling the lanthanum sulfate product to room temperature, and then putting the lanthanum sulfate product into a filter for filtering;
and 4, putting the filtered material into an oven, keeping the temperature of the oven at 100-150 ℃ for 24-36 hours, and crushing the dried material to obtain a finished product of lanthanum sulfate.
Wherein, the molar ratio of the sulfuric acid to the lanthanum oxide in the step 2 is 1:1, 1:0.8, 1:0.65 and 1: 0.4.
Wherein the molar ratio of the sulfuric acid to the lanthanum oxide in the step 2 is 1: 0.65.
Wherein the stirring speed in the step 2 is 80-120R/min when the sulfuric acid is added.
Wherein, the lanthanum sulfate product material in the step 3 is cooled to room temperature of 25-30 degrees, and a centrifuge is adopted for filtration during filtration.
The invention has the beneficial effects that: according to the preparation method of lanthanum sulfate, lanthanum oxide and sulfuric acid are used as raw materials to synthesize lanthanum sulfate, the reaction process is simple, the production cost is low, the production cost can be greatly reduced, and the product quality is stable; meanwhile, the filtrate can be recycled for a plurality of times, no wastewater is discharged, toxic substances such as lead phosphite and the like can be replaced, the national environmental protection requirement is met, and energy is saved.
Detailed Description
Example 1
The preparation method of lanthanum sulfate comprises the following steps:
step 1, adding a proper amount of water into a reaction kettle, heating and stirring the water, keeping the water temperature at 20 ℃, and step 2, sequentially and continuously dripping sulfuric acid and lanthanum oxide into the water, wherein the stirring speed during the addition of the sulfuric acid is 80/min, then continuously stirring uniformly, keeping the temperature of the water at 60 ℃, and carrying out synthetic reaction on the water, the sulfuric acid and the lanthanum oxide to generate lanthanum sulfate, wherein the molar ratio of the sulfuric acid to the lanthanum oxide is 1: 1;
step 3, cooling the lanthanum sulfate product to room temperature of 25 ℃, and then putting the lanthanum sulfate product into a filter for filtering; filtering by adopting a centrifugal machine during filtering;
and 4, putting the filtered material into an oven, keeping the temperature of the oven at 100 ℃, drying for 24 hours, and crushing the dried material to obtain a finished product of lanthanum sulfate.
Example 2
The preparation method of lanthanum sulfate comprises the following steps:
step 1, adding a proper amount of water into a reaction kettle, heating and stirring the water, and keeping the water temperature at 35 ℃;
step 2, sequentially and continuously dripping sulfuric acid and lanthanum oxide into water, wherein the stirring speed of the sulfuric acid is 120R/min, then, the stirring is continuously carried out uniformly, the temperature of the water is kept at 65 ℃, and the water, the sulfuric acid and the lanthanum oxide are subjected to synthetic reaction to generate lanthanum sulfate, wherein the molar ratio of the sulfuric acid to the lanthanum oxide is 1: 0.65;
step 3, cooling the lanthanum sulfate product to room temperature of 30 ℃, then putting the lanthanum sulfate product into a filter for filtering, and filtering by adopting a centrifuge during filtering;
and 4, putting the filtered material into an oven, keeping the temperature of the oven at 150 ℃, drying for 36 hours, and crushing the dried material to obtain a finished product of lanthanum sulfate.
Example 3
The preparation method of lanthanum sulfate comprises the following steps:
step 1, adding a proper amount of water into a reaction kettle, heating and stirring the water, and keeping the water temperature at 35 ℃;
and 2, sequentially and continuously dripping sulfuric acid and lanthanum oxide into water, wherein the stirring speed is 80R/min when the sulfuric acid is added, then the stirring is continuously carried out uniformly, the temperature of the water is kept at 65 ℃, the water, the sulfuric acid and the lanthanum oxide are subjected to synthetic reaction to generate lanthanum sulfate, and the molar ratio of the sulfuric acid to the lanthanum oxide is 1:0.8
Step 3, cooling the lanthanum sulfate product to room temperature of 25 ℃, then putting the lanthanum sulfate product into a filter for filtering, and filtering by adopting a centrifuge during filtering;
and 4, putting the filtered material into an oven, keeping the temperature of the oven at 150 ℃, drying for 30 hours, and crushing the dried material to obtain a finished product of lanthanum sulfate.
The following are the technical indices for lanthanum sulfate prepared in examples 1, 2 and 3:
technical index of lanthanum sulfate
Chemical reaction equation: 3H2SO4+La203→La2(SO4)3+3H20
Quality standard
| Inspection item | Standard requirements |
| Appearance of the product | White powder |
| Content of lanthanum% | 75±1.0 |
| Phosphorous acid% | 10.8±0.5 |
| Heating to reduce weight% | ≤1.5 |
| Fineness (um) D95 | ≤35 |
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. The preparation method of lanthanum sulfate is characterized by comprising the following steps:
step 1, adding a proper amount of water into a reaction kettle, heating and stirring the water, and keeping the water temperature at 20-35 ℃;
step 2, sequentially and continuously dripping sulfuric acid and lanthanum oxide into water, then continuously stirring uniformly, keeping the temperature of the water at 60-65 ℃, and carrying out synthetic reaction on the water, the sulfuric acid and the lanthanum oxide to generate lanthanum sulfate;
step 3, cooling the lanthanum sulfate product to room temperature, and then putting the lanthanum sulfate product into a filter for filtering;
and 4, putting the filtered material into an oven, keeping the temperature of the oven at 100-150 ℃ for 24-36 hours, and crushing the dried material to obtain a finished product of lanthanum sulfate.
2. The method of claim 1, wherein the lanthanum sulfate is obtained by reacting lanthanum sulfate with lanthanum sulfate,
the molar ratio of the sulfuric acid to the lanthanum oxide in the step 2 is 1:1, 1:0.8, 1:0.65 and 1: 0.4.
3. The method of claim 2, wherein the lanthanum sulfate is obtained by reacting lanthanum sulfate with lanthanum sulfate,
the molar ratio of the sulfuric acid to the lanthanum oxide in the step 2 is 1: 0.65.
4. The method of claim 1, wherein the lanthanum sulfate is obtained by reacting lanthanum sulfate with lanthanum sulfate,
the stirring speed in the step 2 is 80-120R/min when the sulfuric acid is added.
5. The method for producing lanthanum phosphite of claim 1,
and (3) cooling the lanthanum sulfate product material to room temperature of 25-30 ℃, and filtering by adopting a centrifuge during filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110400991.2A CN113044872A (en) | 2021-04-14 | 2021-04-14 | Preparation method of lanthanum sulfate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110400991.2A CN113044872A (en) | 2021-04-14 | 2021-04-14 | Preparation method of lanthanum sulfate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445342A (en) * | 2014-11-24 | 2015-03-25 | 益阳鸿源稀土有限责任公司 | Rare-earth salt sulfate and preparation method thereof |
| CN109942396A (en) * | 2019-04-12 | 2019-06-28 | 江苏温塑实业有限公司 | The Preparation Method of lanthanum acetylacetone |
| CN111483991A (en) * | 2020-03-24 | 2020-08-04 | 江苏温塑实业有限公司 | Preparation method of lanthanum phosphite |
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2021
- 2021-04-14 CN CN202110400991.2A patent/CN113044872A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445342A (en) * | 2014-11-24 | 2015-03-25 | 益阳鸿源稀土有限责任公司 | Rare-earth salt sulfate and preparation method thereof |
| CN109942396A (en) * | 2019-04-12 | 2019-06-28 | 江苏温塑实业有限公司 | The Preparation Method of lanthanum acetylacetone |
| CN111483991A (en) * | 2020-03-24 | 2020-08-04 | 江苏温塑实业有限公司 | Preparation method of lanthanum phosphite |
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Application publication date: 20210629 |