CN114604840A - Preparation method of barium pyrophosphate based on barium hydrogen phosphate - Google Patents

Preparation method of barium pyrophosphate based on barium hydrogen phosphate Download PDF

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Publication number
CN114604840A
CN114604840A CN202210253951.4A CN202210253951A CN114604840A CN 114604840 A CN114604840 A CN 114604840A CN 202210253951 A CN202210253951 A CN 202210253951A CN 114604840 A CN114604840 A CN 114604840A
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barium
hydrogen phosphate
phosphoric acid
precipitate
pyrophosphate
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马磊
李海艳
周骏宏
周立国
梁馨亓
韩维玲
郭正仙
王照清
武玉蓉
王祥碧
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Guizhou Shengwei Kaiyang Chemical Co ltd
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Guizhou Shengwei Kaiyang Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/38Condensed phosphates
    • C01B25/42Pyrophosphates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a preparation method of barium pyrophosphate based on barium hydrogen phosphate, which comprises the following steps: s100: preparing solid barium hydrogen phosphate; s200: and calcining the prepared barium hydrogen phosphate in a muffle furnace at the temperature of more than 700 ℃ for more than 20min to obtain the barium pyrophosphate. The invention relates to a synthetic route for further generating barium pyrophosphate by taking phosphoric acid as a phosphorus source and barium salt and barium alkali as barium sources through two-step reaction, namely, firstly generating barium hydrogen phosphate and then dehydrating at high temperature. Because the application value of the barite is not high, if the barite is deeply processed to prepare a fine chemical product, particularly a barium phosphate product prepared by combining barium and phosphorus resources, the barite has obvious significance for exerting the advantages of local resources and improving the economic efficiency.

Description

Preparation method of barium pyrophosphate based on barium hydrogen phosphate
Technical Field
The invention relates to a preparation method of barium pyrophosphate based on barium hydrogen phosphate, belonging to the technical field of chemical industry.
Background
The barite resources and the phosphorite resources in China are rich, wherein the storage amount of the phosphorite resources is the second world, and the quantity of the phosphorite resources in Guizhou province is the second national level. Phosphorite is a raw material of all artificial phosphorus-containing products, including yellow phosphorus, phosphoric acid, phosphate fertilizer, phosphide, organic phosphorus and the like, has an important position in national economy, is a non-renewable resource and has great strategic value. The barite resource of Guizhou province is rich, accounts for one third of the total reserves of the whole country, has the characteristics of high density, difficult water and acid dissolution, no toxicity, no magnetism, easy radiation absorption, good filling property, stable thermodynamic property and the like, and is widely applied to more than ten industries such as chemical industry, building materials, metallurgy, textile, electronics, building materials, medicine and the like.
Barium pyrophosphate is a novel barium-containing phosphorus-containing compound, and has special use effect due to unique chemical properties. For example, in the production process of calcium phosphate ceramics, the bending strength can be improved when a small amount of pyrophosphoric acid is added to the raw materials, the mechanical strength of the catalyst can be improved by adding barium pyrophosphate as a catalyst in the synthesis of triethylene diamine, the service life of the catalyst can be prolonged, the use of barium pyrophosphate as a carrier has a good effect in the preparation of 2, 3-pentanedione, and the research shows that barium pyrophosphate may be a promising blue-emitting phosphor of a near-ultraviolet light-emitting diode. There are few reports on the production of barium pyrophosphate, and the preparation method which can be found lacks detailed description, and only has a general idea and no specific steps.
Disclosure of Invention
The invention aims to provide a preparation method of barium pyrophosphate based on barium hydrogen phosphate, which is a synthetic route for further generating barium pyrophosphate by using phosphoric acid as a phosphorus source and barium salt and barium alkali as barium sources through two-step reaction, namely firstly generating barium hydrogen phosphate and then dehydrating at high temperature.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of barium pyrophosphate based on barium hydrogen phosphate comprises the following steps: s100: preparing solid barium hydrogen phosphate; s200: and calcining the prepared barium hydrogen phosphate in a muffle furnace at the temperature of more than 700 ℃ for more than 20min to obtain the barium pyrophosphate.
In the method for preparing barium pyrophosphate based on barium hydrogen phosphate, step S100 includes the following steps:
adding barium carbonate into a phosphoric acid solution to prepare barium hydrogen phosphate, washing the precipitated barium hydrogen phosphate, and drying in a drying oven to obtain solid barium hydrogen phosphate.
In the foregoing method for preparing barium pyrophosphate based on barium hydrogen phosphate, step S100 further includes the following steps: weighing 16.99g of barium carbonate, placing the barium carbonate in a 250ml beaker, adding 9.93g of 85% phosphoric acid diluted to 100ml, stirring while adding, then heating and stirring for 45min by using a magnetic stirrer, washing for 3-4 times after precipitation, and drying in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
In the method for preparing barium pyrophosphate based on barium hydrogen phosphate, step S100 includes the following steps: weighing Ba (OH)2·8H2And O and phosphoric acid are mixed and stirred to separate out a precipitate, and the precipitate is washed and dried in an oven to obtain solid barium hydrogen phosphate.
In the foregoing method for preparing barium pyrophosphate based on barium hydrogen phosphate, step S100 further includes the following steps: weigh 27.16g Ba (OH)2·8H2And O, 9.93g of 85% phosphoric acid, putting the phosphoric acid into a 250ml beaker, adding 9.93g of 85% diluted phosphoric acid into the beaker to 100ml of the phosphoric acid, stirring the phosphoric acid while adding the phosphoric acid, heating and stirring the mixture for 45min by using a magnetic stirrer, separating out a precipitate, washing the precipitate for 4-5 times, and drying the precipitate in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
The above-mentioned one based on hydrogen phosphateIn the method for producing barium pyrophosphate of barium, the step S100 includes the following steps: weighing of BaCl 2H2O is prepared into a solution, and NaH is weighed2PO4·2H2And preparing the solution of O, mixing the two solutions, washing the precipitate after precipitation, and drying in an oven to obtain the solid barium hydrogen phosphate.
In the method for preparing barium pyrophosphate based on barium hydrogen phosphate, step S100 includes the following steps: weighing of BaCl 2H2O104.69 g, prepared into a 1L solution; weighing NaH2PO4·2H2O133.73 g, prepared into a 1L solution; and (3) mixing 50ml of the two solutions, adding the two solutions while stirring, heating and stirring for 45min by using a magnetic stirrer, washing the precipitate for 3-4 times after the precipitate is separated out, and drying in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
Compared with the prior art, the invention takes phosphoric acid as a phosphorus source and barium salt and barium alkali as barium sources, and the synthesis route further generates barium pyrophosphate through two-step reaction, namely, firstly generates barium hydrogen phosphate and then dehydrates at high temperature. Because the application value of the barite is not high, if the barite is deeply processed to prepare a fine chemical product, particularly a barium phosphate product prepared by combining barium and phosphorus resources, the barite has obvious significance for exerting the advantages of local resources and improving the economic efficiency. 1. Aiming at the problems that the research on the preparation of barium pyrophosphate is rare and cannot meet the requirements of new material application and development trend in the future, the invention researches a synthetic route which uses phosphoric acid as a phosphorus source and barium sources such as barium salt, barium alkali and the like, firstly prepares barium hydrogen phosphate, and then dehydrates at high temperature to obtain barium pyrophosphate, and systematically and completely researches the synthesis conditions and influencing factors. 2. During the research, it was found that the precipitate formed after the phosphate and barium ions met, unlike other common phosphates, barium hydrogen phosphate more easily appears as a dominant phase and preferentially precipitates out of solution, and barium dihydrogen phosphate or barium tribasic phosphate is not easily formed in acidic (even if pH 1.49) or alkaline solutions (even if pH 13.15). This finding is not reported. 3. Further studies have found that phosphate and barium ions readily form barium sodium phosphate compounds after the solution pH is greater than 7 in the presence of sodium ions, and that tribasic barium phosphate is also difficult to form under alkaline conditions (pH 12.69) instead of barium phosphate dibasic. That is, the ratio of phosphorus to barium is 1: the compound of 1 is more readily formed under the conditions of this experiment. This finding is not reported.
Drawings
FIG. 1 is an XRD pattern of barium pyrophosphate;
FIG. 2 is an XRD pattern of calcined barium hydrogen phosphate at different temperatures;
FIG. 3 is an XRD pattern of barium hydrogen phosphate calcined at different times;
FIG. 4 is an XRD pattern of the reaction of barium carbonate and phosphoric acid;
FIG. 5 is a graph of the stability of the intermediate barium hydrogen phosphate formed under various pH conditions.
The invention is further described with reference to the following figures and detailed description.
Detailed Description
Example 1 of the invention: a preparation method of barium pyrophosphate based on barium hydrogen phosphate comprises the following steps:
s100: weighing 16.99g of barium carbonate, placing the barium carbonate in a 250ml beaker, adding 9.93g of 85% phosphoric acid diluted to 100ml, stirring while adding, then heating and stirring for 45min by using a magnetic stirrer, washing for 3-4 times after precipitation, and drying in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
S200: and calcining the prepared barium hydrogen phosphate in a muffle furnace at the temperature of more than 700 ℃ for more than 20min to obtain the barium pyrophosphate. The barium pyrophosphate prepared by the above example had a purity of 99.1%.
Example 2: a preparation method of barium pyrophosphate based on barium hydrogen phosphate comprises the following steps:
s100: weigh 27.16g Ba (OH)2·8H2And O, 9.93g of 85% phosphoric acid, putting the phosphoric acid into a 250ml beaker, adding 9.93g of 85% diluted phosphoric acid into the beaker to 100ml of the phosphoric acid, stirring the phosphoric acid while adding the phosphoric acid, heating and stirring the mixture for 45min by using a magnetic stirrer, separating out a precipitate, washing the precipitate for 4-5 times, and drying the precipitate in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
S200: and calcining the prepared barium hydrogen phosphate in a muffle furnace at the temperature of more than 700 ℃ for more than 20min to obtain the barium pyrophosphate. The barium pyrophosphate prepared by the above example had a purity of 99.7%.
Example 3: a preparation method of barium pyrophosphate based on barium hydrogen phosphate comprises the following steps:
s100: weighing of BaCl 2H2O104.69 g, prepared into a 1L solution; weighing NaH2PO4·2H2O133.73 g, prepared into a 1L solution; and (3) mixing 50ml of the two solutions, adding the two solutions while stirring, heating and stirring for 45min by using a magnetic stirrer, washing the precipitate for 3-4 times after the precipitate is separated out, and drying in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
S200: and calcining the prepared barium hydrogen phosphate in a muffle furnace at the temperature of more than 700 ℃ for more than 20min to obtain the barium pyrophosphate. The barium pyrophosphate prepared by the above example had a purity of 99.4%.
FIGS. 1 to 5 are XRD patterns of barium pyrophosphate in sequence; XRD patterns of calcined barium hydrogen phosphate at different temperatures; calcining the XRD pattern of the barium hydrogen phosphate at different times; XRD pattern of barium carbonate and phosphoric acid reaction; the stability profile was developed for the intermediate barium hydrogen phosphate at different pH conditions. The purity of the barium pyrophosphate prepared by adopting the embodiment is between 99.1% and 99.7%.

Claims (7)

1. A preparation method of barium pyrophosphate based on barium hydrogen phosphate is characterized by comprising the following steps:
s100: preparing solid barium hydrogen phosphate;
s200: and calcining the prepared barium hydrogen phosphate in a muffle furnace at the temperature of more than 700 ℃ for more than 20min to obtain the barium pyrophosphate.
2. The method of claim 1, wherein the step S100 comprises the following steps:
adding barium carbonate into a phosphoric acid solution to prepare barium hydrogen phosphate, washing the precipitated barium hydrogen phosphate, and drying in a drying oven to obtain solid barium hydrogen phosphate.
3. The method of claim 2, wherein the step S100 further comprises the following steps: weighing 16.99g of barium carbonate, placing the barium carbonate in a 250ml beaker, adding 9.93g of 85% phosphoric acid diluted to 100ml, stirring while adding, then heating and stirring for 45min by using a magnetic stirrer, washing for 3-4 times after precipitation, and drying in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
4. The method of claim 1, wherein the step S100 comprises the following steps:
weighing Ba (OH)2·8H2And O and phosphoric acid are mixed and stirred to separate out a precipitate, and the precipitate is washed and dried in an oven to obtain solid barium hydrogen phosphate.
5. The method of claim 4, wherein the step S100 further comprises the following steps: weigh 27.16g Ba (OH)2·8H2And O, 9.93g of 85% phosphoric acid, putting the phosphoric acid into a 250ml beaker, adding 9.93g of 85% diluted phosphoric acid into the beaker to 100ml of the phosphoric acid, stirring the phosphoric acid while adding the phosphoric acid, heating and stirring the mixture for 45min by using a magnetic stirrer, separating out a precipitate, washing the precipitate for 4-5 times, and drying the precipitate in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
6. The method of claim 1, wherein the step S100 comprises the following steps:
weighing of BaCl 2H2Preparing O into solution, weighing NaH2PO4·2H2And preparing the solution of O, mixing the two solutions, washing the precipitate after precipitation, and drying in an oven to obtain the solid barium hydrogen phosphate.
7. The method of claim 6, wherein the step S100 comprises the following steps:
weighing of BaCl 2H2O104.69 g, prepared into a 1L solution; weighing NaH2PO4·2H2O133.73 g, prepared into a 1L solution; and (3) mixing 50ml of the two solutions, adding the two solutions while stirring, heating and stirring for 45min by using a magnetic stirrer, washing the precipitate for 3-4 times after the precipitate is separated out, and drying in an oven at 150 ℃ to obtain solid barium hydrogen phosphate.
CN202210253951.4A 2022-03-15 2022-03-15 Preparation method of barium pyrophosphate based on barium hydrogen phosphate Pending CN114604840A (en)

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Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA342224A (en) * 1934-06-12 Reimann Albert Neutral sodium pyrophosphate
GB742623A (en) * 1952-09-15 1955-12-30 Chem Fab Budenheim Ag Production of pyrophosphates and polyphosphates
GB744576A (en) * 1952-12-15 1956-02-08 Chem Fab Budenheim Ag Production of alkali metal pyrophosphates and triphosphates of low bulk weight
CH332125A (en) * 1952-12-15 1958-08-31 Chem Fab Budenheim Ag Process for the preparation of alkali pyro- or alkali tripolyphosphate of low bulk density
USB471221I5 (en) * 1974-05-20 1976-01-13
US3975308A (en) * 1975-02-07 1976-08-17 The Carborundum Company Preparation of pyrophosphates
CN101723342A (en) * 2009-10-28 2010-06-09 广东光华化学厂有限公司 Method for preparing electronic grade high-purity potassium permanganate
CN102153062A (en) * 2011-01-30 2011-08-17 广东光华科技股份有限公司 Method for preparing electronic grade high-purity zinc pyrophosphate
CN103058162A (en) * 2012-12-29 2013-04-24 广东光华科技股份有限公司 Preparation method for electronic grade high-purity copper pyrophosphate
US20130294994A1 (en) * 2010-09-09 2013-11-07 Adeka Corporation Method for producing pyrophosphate
CN107051557A (en) * 2017-06-05 2017-08-18 西华师范大学 A kind of barium pyrophosphate load cesium-promoted catalyst and preparation method thereof, application
CN107697895A (en) * 2017-09-13 2018-02-16 苏州安锰新能源科技有限公司 A kind of nanoporous manganese pyrophosphate and preparation method thereof
CN109231180A (en) * 2017-12-19 2019-01-18 江苏省国盛稀土有限公司 A method of preparing high-purity phosphoric acid dihydro barium
JP2020011869A (en) * 2018-07-19 2020-01-23 Dowaエレクトロニクス株式会社 Method for producing germanium pyrophosphate
CN112875669A (en) * 2021-01-16 2021-06-01 黔南民族师范学院 Method for preparing barium metaphosphate by decomposing barite with ammonium dihydrogen phosphate

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA342224A (en) * 1934-06-12 Reimann Albert Neutral sodium pyrophosphate
GB742623A (en) * 1952-09-15 1955-12-30 Chem Fab Budenheim Ag Production of pyrophosphates and polyphosphates
GB744576A (en) * 1952-12-15 1956-02-08 Chem Fab Budenheim Ag Production of alkali metal pyrophosphates and triphosphates of low bulk weight
CH332125A (en) * 1952-12-15 1958-08-31 Chem Fab Budenheim Ag Process for the preparation of alkali pyro- or alkali tripolyphosphate of low bulk density
USB471221I5 (en) * 1974-05-20 1976-01-13
US3975308A (en) * 1975-02-07 1976-08-17 The Carborundum Company Preparation of pyrophosphates
CN101723342A (en) * 2009-10-28 2010-06-09 广东光华化学厂有限公司 Method for preparing electronic grade high-purity potassium permanganate
US20130294994A1 (en) * 2010-09-09 2013-11-07 Adeka Corporation Method for producing pyrophosphate
CN102153062A (en) * 2011-01-30 2011-08-17 广东光华科技股份有限公司 Method for preparing electronic grade high-purity zinc pyrophosphate
CN103058162A (en) * 2012-12-29 2013-04-24 广东光华科技股份有限公司 Preparation method for electronic grade high-purity copper pyrophosphate
CN107051557A (en) * 2017-06-05 2017-08-18 西华师范大学 A kind of barium pyrophosphate load cesium-promoted catalyst and preparation method thereof, application
CN107697895A (en) * 2017-09-13 2018-02-16 苏州安锰新能源科技有限公司 A kind of nanoporous manganese pyrophosphate and preparation method thereof
CN109231180A (en) * 2017-12-19 2019-01-18 江苏省国盛稀土有限公司 A method of preparing high-purity phosphoric acid dihydro barium
JP2020011869A (en) * 2018-07-19 2020-01-23 Dowaエレクトロニクス株式会社 Method for producing germanium pyrophosphate
CN112875669A (en) * 2021-01-16 2021-06-01 黔南民族师范学院 Method for preparing barium metaphosphate by decomposing barite with ammonium dihydrogen phosphate

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Application publication date: 20220610