CN109231180A - A method of preparing high-purity phosphoric acid dihydro barium - Google Patents
A method of preparing high-purity phosphoric acid dihydro barium Download PDFInfo
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- CN109231180A CN109231180A CN201711378807.9A CN201711378807A CN109231180A CN 109231180 A CN109231180 A CN 109231180A CN 201711378807 A CN201711378807 A CN 201711378807A CN 109231180 A CN109231180 A CN 109231180A
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- barium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/322—Preparation by neutralisation of orthophosphoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to technical field of chemical purification, it is related to a kind of method for preparing high-purity phosphoric acid dihydro barium, step includes the electron-level phosphoric acid that 3~10mol/L is added in a kettle, then the barium carbonate or barium hydroxide with amounts of substances such as phosphoric acid is added, suspension is filtered after fully reacting, obtains barium hydrogen phosphate sediment；After gained barium hydrogen phosphate sediment drying and dewatering, high concentration phosphorus acid solution is added, barium dihydrogen phosphate crystallization is precipitated, filtering obtains biphosphate crystal of barium and mother liquor；Gained biphosphate crystal of barium is eluted to the attached acid for removing surface entrainment with water, obtains high-purity phosphoric acid dihydro barium.The present invention utilizes H2PO4 ‑Common-ion effect, crystallize out barium dihydrogen phosphate directly from mother liquor, obtained barium dihydrogen phosphate purity is high, the concentration of each non-ferrous metal element impurity is in 5ppm hereinafter, equipment investment needed for technique is small, effect is good, is suitble to Large scale processes application.
Description
Technical field
The present invention relates to technical field of chemical purification, in particular to it is a kind of it is high-efficient, at low cost, easy to use, environment is friendly
The good method for preparing high-purity phosphoric acid dihydro barium.
Background technique
High-purity phosphoric acid dihydro barium is one of high-purity phosphoric acid dihydric salt, common to do some precision machineries, measuring instrument
Host glass etc. is the important source material of laser glass in high power laser.The conventional method for preparing high-purity phosphoric acid dihydro barium is
By barium carbonate or barium hydroxide and phosphatase reaction, barium dihydrogen phosphate solution is generated.Then by the solution decrease temperature crystalline, from solution
Biphosphate crystal of barium is precipitated.Barium hydrogen phosphate, and crystalline mother solution are usually mixed in the biphosphate crystal of barium that this method obtains
Generally requiring to be concentrated by evaporation can just continue to use, and cause to prepare biphosphate crystal of barium higher cost, industrial production can not receive.
It is therefore desirable to provide a kind of preparation method of more economical environmental protection to solve problem above.
Summary of the invention
The purpose of the invention is to provide a kind of economic and environment-friendly method for preparing high-purity phosphoric acid dihydro barium.
A kind of method for preparing high-purity phosphoric acid dihydro barium of the present invention, includes the following steps:
Step is 1.: the electron-level phosphoric acid of 3~10mol/L being added in a kettle, the amount with substances such as phosphoric acid is then added
Barium carbonate or barium hydroxide, suspension is filtered after fully reacting, obtains barium hydrogen phosphate sediment；
Step is 2.: after step 1. gained barium hydrogen phosphate sediment drying and dewatering, high concentration phosphorus acid solution, precipitation of phosphorus is added
The crystallization of acid dihydride barium, filtering obtain biphosphate crystal of barium and mother liquor；
Step is 3.: by step, 2. gained biphosphate crystal of barium is eluted with water and removes the attached acid of surface entrainment, is obtained high-purity
Barium dihydrogen phosphate.
Specifically, step 1. in reaction condition be stirring under, 25~90 DEG C of reaction temperature, the reaction time control exists
1~5h.
Specifically, step 2. middle and high concentration phosphoric acid substance withdrawl syndrome control in 6~12mol/L, the phosphoric acid hydrogen of addition
The control of the ratio between amount of substance of phosphoric acid is in 1~1.7:3 in barium and solution.
Specifically, step 2. in reaction condition be stirring under, 60~95 DEG C of reaction temperature, 3~6h of reaction time.
Specifically, 2. resulting mother liquor mends reuse after phosphoric acid to step.
The invention has the beneficial effects that:
1, the present invention utilizes H2PO4 -Common-ion effect, crystallize out barium dihydrogen phosphate directly from mother liquor, obtain
Barium dihydrogen phosphate purity is high, the concentration of each non-ferrous metal element impurity is in 5ppm hereinafter, equipment investment needed for technique is small, effect
Good, suitable Large scale processes application.
2, barium dihydrogen phosphate is directly crystallized out from mother liquor at ambient temperature or elevated temperature, without cooling, is avoided using drop
Energy loss caused by temperature crystallization.
3, mother liquor can return to the new a collection of barium hydrogen phosphate of processing after adding phosphoric acid, and mother liquor can be realized without being concentrated by evaporation
It recycles, it is environment friendly and pollution-free.
Detailed description of the invention
Fig. 1 is the general flow chart of present invention process.
Fig. 2 be 1 step of embodiment 1. gained barium hydrogen phosphate X ray diffracting spectrum.
Fig. 3 be 1 step of embodiment 3. gained barium dihydrogen phosphate X ray diffracting spectrum.
Specific embodiment
As shown in Figure 1, a kind of method for preparing high-purity phosphoric acid dihydro barium, includes the following steps:
Step is 1.: the electron-level phosphoric acid of 2~9mol/L being added in a kettle, is then added and the amounts of substances such as phosphoric acid
Barium carbonate or barium hydroxide are filtered suspension after fully reacting, obtain barium hydrogen phosphate sediment；
Step is 2.: after step 1. gained barium hydrogen phosphate sediment drying and dewatering, high concentration phosphorus acid solution, precipitation of phosphorus is added
The crystallization of acid dihydride barium, filtering obtain biphosphate crystal of barium and mother liquor；
Step is 3.: by step, 2. gained biphosphate crystal of barium is eluted with water and removes the attached acid of surface entrainment, is obtained high-purity
Barium dihydrogen phosphate.
Invention is further described in detail combined with specific embodiments below.
Embodiment 1:
Electron-level phosphoric acid (concentration 85%) 100kg is added in a kettle, high purity water is added and is diluted to phosphoric acid concentration
3mol/L is stirred evenly and solution temperature is risen to 60 DEG C, high-pruity barium carbonate powder 170kg is then slowly added into, in this process
Middle key reaction are as follows:
BaCO3+H3PO4=BaHPO4+H2O+CO2↑
During the addition process, phosphoric acid is all to be in excessive state, therefore the carbon dioxide generated will escape at once, is reduced
The presence of bicarbonate ion.The barium hydrogen phosphate suspension that reaction obtains is filtered after reaction 1h, after filter cake drying
To solid about 100kg, solid is sampled and carries out X-ray diffraction detection, as a result sees Fig. 2.Top indicates barium hydrogen phosphate in figure, and
The content of impurity is more.
Electron-level phosphoric acid (concentration 85%) 250kg is added in a kettle, high purity water is added and is adjusted to phosphoric acid concentration
12mol/L is stirred evenly and solution temperature is risen to 95 DEG C, is slowly added to barium hydrogen phosphate sediment 100kg, is filtered after stirring 3h
Biphosphate crystal of barium 110kg and mother liquor are obtained, in the process key reaction are as follows:
BaHPO4+H3PO4=Ba (H2PO4)2
Obtained crystal can remove the attached acid of surface entrainment through the elution of a small amount of water, sample to crystal and carry out X-ray diffraction
Detection, is as a result shown in Fig. 3.Top indicates barium dihydrogen phosphate in figure, and impurity obviously tails off, each non-ferrous metal element impurity it is dense
Degree is in 5ppm or less.
Embodiment 2:
Electron-level phosphoric acid (concentration 85%) 100kg is added in a kettle, high purity water is added and is diluted to phosphoric acid concentration
5mol/L is stirred evenly and solution temperature is risen to 90 DEG C, is then slowly added into high-purity barium hydroxide octahydrate 274kg, is obtained
Key reaction in the process are as follows:
Ba(OH)2·8H2O+H3PO4=BaHPO4+10H2O
The barium hydrogen phosphate suspension that reaction obtains is filtered after reaction 3h, obtains solid about 130kg after filter cake drying.
Electron-level phosphoric acid (concentration 85%) 150kg is added in a kettle, appropriate high purity water is added and adjusts phosphoric acid concentration
It to 6mol/L, stirs and solution temperature is risen to 80 DEG C, be slowly added to barium hydrogen phosphate sediment 130kg, filtered after stirring 6h
To biphosphate crystal of barium 147kg and mother liquor, obtained crystal can remove the attached acid of surface entrainment through the elution of a small amount of water.
Embodiment 3:
Electron-level phosphoric acid (concentration 85%) 100kg is added in a kettle, high purity water is added and is diluted to phosphoric acid concentration
10mol/L is stirred evenly and solution temperature is maintained at 25 DEG C, is then slowly added into high-pruity barium carbonate powder 170kg, reacts 5h
The barium hydrogen phosphate suspension that reaction obtains is filtered afterwards, obtains solid about 155kg after filter cake drying.
Electron-level phosphoric acid (concentration 85%) 320kg is added in a kettle, high purity water is added and is adjusted to phosphoric acid concentration
12mol/L is stirred evenly and solution temperature is risen to 60 DEG C, is slowly added to barium hydrogen phosphate sediment 155kg, is filtered after stirring 4h
Biphosphate crystal of barium 168kg and mother liquor are obtained, obtained crystal can remove the attached acid of surface entrainment through the elution of a small amount of water.
Present invention utilizes H2PO4 -Common-ion effect, make barium dihydrogen phosphate directly at ambient temperature or elevated temperature from mother liquor
It crystallizes out, without cooling, avoids using energy loss caused by decrease temperature crystalline.Equipment investment needed for technique is small, effect is good,
It is suitble to Large scale processes application.
Mother liquor in Examples 1 to 3 is back to use in crystallization next time after can supplementing phosphoric acid, is not wasted.Mother liquor without
It need to be concentrated by evaporation can be realized and recycle, it is environment friendly and pollution-free.
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these belong to protection model of the invention
It encloses.
Claims (5)
1. a kind of method for preparing high-purity phosphoric acid dihydro barium, it is characterised in that the following steps are included:
Step is 1.: the electron-level phosphoric acid of 3~10mol/L being added in a kettle, the carbon with amounts of substances such as phosphoric acid is then added
Sour barium or barium hydroxide are filtered suspension after fully reacting, obtain barium hydrogen phosphate sediment；
Step is 2.: after step 1. gained barium hydrogen phosphate sediment drying and dewatering, high concentration phosphorus acid solution is added, di(2-ethylhexyl)phosphate is precipitated
The crystallization of hydrogen barium, filtering obtain biphosphate crystal of barium and mother liquor；
Step is 3.: by step, 2. gained biphosphate crystal of barium is eluted with water and removes the attached acid of surface entrainment, obtains high-purity phosphoric acid
Dihydro barium.
2. a kind of method for preparing high-purity phosphoric acid dihydro barium according to claim 1, it is characterised in that: step 1. in it is anti-
Answering condition is 25~90 DEG C of reaction temperature under stirring, and the reaction time controls in 1~5h.
3. a kind of method for preparing high-purity phosphoric acid dihydro barium according to claim 1, it is characterised in that: step 2. in it is highly concentrated
The substance withdrawl syndrome for spending phosphoric acid controls the ratio between the amount of substance of the phosphoric acid in 6~12mol/L, the barium hydrogen phosphate and solution of addition
Control is in 1~1.7:3.
4. a kind of method for preparing high-purity phosphoric acid dihydro barium according to claim 1, it is characterised in that: step 2. in it is anti-
Answering condition is 60~95 DEG C of reaction temperature under stirring, 3~6h of reaction time.
5. a kind of method for preparing high-purity phosphoric acid dihydro barium according to claim 1, it is characterised in that: step is 2. resulting
Mother liquor mends reuse after phosphoric acid.
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| CN201711378807.9A CN109231180B (en) | 2017-12-19 | 2017-12-19 | Method for preparing high-purity barium dihydrogen phosphate |
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| CN201711378807.9A CN109231180B (en) | 2017-12-19 | 2017-12-19 | Method for preparing high-purity barium dihydrogen phosphate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362241A (en) * | 2020-05-15 | 2020-07-03 | 南通太洋高新材料科技有限公司 | Preparation method of optical-grade barium dihydrogen phosphate |
| CN114604839A (en) * | 2022-03-15 | 2022-06-10 | 贵州胜威凯洋化工有限公司 | Preparation method of barium pyrophosphate |
| CN114604840A (en) * | 2022-03-15 | 2022-06-10 | 贵州胜威凯洋化工有限公司 | Preparation method of barium pyrophosphate based on barium hydrogen phosphate |
| CN115490221A (en) * | 2022-09-26 | 2022-12-20 | 青岛天尧新材料有限公司 | Method for producing barium metaphosphate by taking barium carbonate as raw material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1472441A1 (en) * | 1987-01-06 | 1989-04-15 | Казахский Научно-Исследовательский И Проектный Институт Фосфорной Промышленности | Method of producing single-substituted barium phosphate |
| CN1800000A (en) * | 2004-12-31 | 2006-07-12 | 山西超新金属材料有限公司 | Barium metaphosphorate production process |
| CN106006596A (en) * | 2016-08-03 | 2016-10-12 | 广东广试试剂科技有限公司 | Preparation method of highly-pure barium dihydrogen phosphate |
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2017
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Patent Citations (3)
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| SU1472441A1 (en) * | 1987-01-06 | 1989-04-15 | Казахский Научно-Исследовательский И Проектный Институт Фосфорной Промышленности | Method of producing single-substituted barium phosphate |
| CN1800000A (en) * | 2004-12-31 | 2006-07-12 | 山西超新金属材料有限公司 | Barium metaphosphorate production process |
| CN106006596A (en) * | 2016-08-03 | 2016-10-12 | 广东广试试剂科技有限公司 | Preparation method of highly-pure barium dihydrogen phosphate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362241A (en) * | 2020-05-15 | 2020-07-03 | 南通太洋高新材料科技有限公司 | Preparation method of optical-grade barium dihydrogen phosphate |
| CN114604839A (en) * | 2022-03-15 | 2022-06-10 | 贵州胜威凯洋化工有限公司 | Preparation method of barium pyrophosphate |
| CN114604840A (en) * | 2022-03-15 | 2022-06-10 | 贵州胜威凯洋化工有限公司 | Preparation method of barium pyrophosphate based on barium hydrogen phosphate |
| CN115490221A (en) * | 2022-09-26 | 2022-12-20 | 青岛天尧新材料有限公司 | Method for producing barium metaphosphate by taking barium carbonate as raw material |
| CN115490221B (en) * | 2022-09-26 | 2024-03-19 | 青岛天尧新材料有限公司 | Method for producing barium metaphosphate by taking barium carbonate as raw material |
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| CN109231180B (en) | 2022-04-05 |
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