CN111422849A - Preparation method of optical-grade calcium metaphosphate - Google Patents
Preparation method of optical-grade calcium metaphosphate Download PDFInfo
- Publication number
- CN111422849A CN111422849A CN202010415023.4A CN202010415023A CN111422849A CN 111422849 A CN111422849 A CN 111422849A CN 202010415023 A CN202010415023 A CN 202010415023A CN 111422849 A CN111422849 A CN 111422849A
- Authority
- CN
- China
- Prior art keywords
- calcium
- exchange resin
- phosphate solution
- calcination
- metaphosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- C01B25/38—Condensed phosphates
- C01B25/44—Metaphosphates
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- 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
-
- 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
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The technical scheme of the invention provides a preparation method of optical-grade calcium metaphosphate, which comprises the following steps: reacting a calcium source with phosphoric acid and water according to a certain proportion under the conditions of heating and pressurizing to obtain a crude calcium dihydrogen phosphate solution, wherein the calcium source is selected from calcium hydroxide or calcium oxide; adjusting the concentration of the crude calcium dihydrogen phosphate solution and enabling the crude calcium dihydrogen phosphate solution to pass through ion exchange resin to remove nonferrous metals and impurity ions; evaporating and concentrating the solution after ion exchange resin, and concentrating to more than 25%; carrying out first clean calcination to remove free water and structural water to obtain calcium metaphosphate intermediate powder; and carrying out secondary clean calcination to obtain the optical grade calcium metaphosphate finished product. The preparation method of the technical scheme of the invention has strong adaptability to the raw material calcium hydroxide or calcium oxide, the prepared calcium metaphosphate has high purity, all indexes meet the requirements of the raw materials of optical glass and laser glass, and a key high-purity raw material is provided for the industrial production of the laser glass and the civil optical glass.
Description
Technical Field
The invention relates to the field of fine inorganic phosphorus chemical industry, in particular to a preparation method of optical-grade calcium metaphosphate.
Background
Metaphosphate is the most stable phosphate among dibasic phosphates, and is a basic raw material for the production of phosphate glass. The high-purity metaphosphate has excellent light transmittance, so that the metaphosphate can be used as an important raw material of laser glass in a high-power laser (such as national scientific engineering-Shenguang plan) and also can be used as an important raw material of some advanced optical equipment such as camera lenses, high-definition cameras, smart phone lenses and mobile phone panel substrates. The transition metals of Fe, Co, Ni and the like can cause strong absorption of metaphosphate glass in the near ultraviolet to infrared regions, and the optical performance of the glass is influenced. Therefore, the preparation of high purity metaphosphate raw material becomes the key to the manufacture of high performance laser glass.
Although China is a large country for producing phosphorus chemical industry, the development of high-additive and fine phosphorus chemical industry products is lagged, and the competitiveness of the international market is lacked. In view of technical blockade of international peers, the economic benefits of enterprises can be improved only by independent innovation, deep development of refined phosphorus chemical products is enhanced, high-tech content of the products is improved, and additional value of the products is improved.
Disclosure of Invention
In view of the above-mentioned current state of the art, the technical problem to be solved by the present invention is to provide a method for preparing optical grade calcium metaphosphate, wherein the main index of the prepared calcium metaphosphate can meet the requirement of manufacturing optical glass and laser glass.
In order to solve the technical problems, the technical scheme of the invention provides a preparation method of optical-grade calcium metaphosphate, which comprises the following steps:
1) reacting a calcium source with phosphoric acid and water according to a certain proportion under the conditions of heating and pressurizing to obtain a crude calcium dihydrogen phosphate solution, wherein the calcium source is selected from calcium hydroxide or calcium oxide;
2) adjusting the concentration of the crude calcium dihydrogen phosphate solution and enabling the crude calcium dihydrogen phosphate solution to pass through ion exchange resin to remove nonferrous metals and impurity ions;
3) evaporating and concentrating the solution after ion exchange resin, and concentrating to more than 25%;
4) carrying out first clean calcination to remove free water and structural water to obtain calcium metaphosphate intermediate powder;
5) and carrying out secondary clean calcination to obtain the optical grade calcium metaphosphate finished product.
Preferably, the molar ratio of the calcium source to the phosphoric acid is 1 (1.97-2.03), and the mass ratio of the phosphoric acid to the water is 1 (2.1-3.5). More preferably, the molar ratio of the calcium source to the phosphoric acid is 1 (1.985-2.015), and the mass ratio of the phosphoric acid to the water is 1 (2.2-2.9).
Preferably, in the step 1), the reaction temperature is 120-140 ℃, the reaction pressure is 0.25-0.5 MPa, and the reaction time is 3-7 h. Further preferably, the reaction temperature is 125-135 ℃, the reaction pressure is 0.3-0.45 MPa, and the reaction time is 4-6 h.
Preferably, the concentration of the crude monocalcium phosphate solution is adjusted to 8% -16%, the flow rate of the crude monocalcium phosphate solution passing through the ion exchange resin is 1L/min-5L/min, further, the concentration of the crude monocalcium phosphate solution is adjusted to 9% -14%, and the flow rate of the crude monocalcium phosphate solution passing through the ion exchange resin is 2L/min-4L/min.
Preferably, the ion exchange resin comprises cation exchange resin and anion exchange resin, the cation exchange resin comprises one or more of 732, D401, D402, D405, IONRISI 1600 and IONRISI 35, and the anion exchange resin comprises one or more of 201 × 7, D201, D202, D407 and IONRISI IRA 400.
Preferably, in the step 3), the concentration is 25 to 30 percent. More preferably, the concentration is 26-28%.
Preferably, the concentrated calcium dihydrogen phosphate solution enters a spray calcining tower at the flow rate of 5L-13L/min for first clean calcination, wherein the air inlet temperature is 720-800 ℃, the upper section temperature of the tower body is 690-770 ℃, the middle section temperature of the tower body is 660-740 ℃, the lower section temperature of the tower body is 630-705 ℃, and the air outlet temperature is 400-475 ℃.
And further, the concentrated calcium dihydrogen phosphate solution enters a spray calcining tower at the flow rate of 7L/min-10L/min for first clean calcination, wherein the air inlet temperature is 740-780 ℃, the upper section temperature of the tower body is 710-755 ℃, the middle section temperature of the tower body is 680-725 ℃, the lower section temperature of the tower body is 655-690 ℃, and the air outlet temperature is 420-450 ℃.
In the process of spray calcination, in order to ensure that materials are not polluted, clean calcination is required to be ensured, only an indirect heating mode is adopted, and the following problems are that the highest air inlet temperature of a spray calcination tower can only reach 780-800 ℃ (the tower body temperature can only reach 700-740 ℃), and in the working condition of instantaneous calcination dehydration, the temperature section is difficult to completely dehydrate for the calcination of calcium metaphosphate, 97% of calcium dihydrogen phosphate structural water can be removed at most, and higher lasting temperature and further calcination equipment are required to remove the final trace structural water. Therefore, the invention adopts a secondary calcination method, and carries out secondary clean calcination in an electric furnace, wherein the calcination temperature of the electric furnace is 760-860 ℃, and the calcination time is 4-10 h.
Furthermore, the calcining temperature of the electric furnace is 790-840 ℃, and the calcining time is 6-9 h. The hearth is lined with high-purity corundum or high-purity quartz material.
The preparation method of the optical grade calcium metaphosphate provided by the technical scheme of the invention has the following beneficial effects: the method has strong adaptability to the raw materials of calcium hydroxide or calcium oxide, adopts a mode of removing impurities by an ion exchange method, indirectly heating, cleaning, spraying and calcining and combining with the cleaning and calcining of a high-temperature electric furnace, and the prepared calcium metaphosphate has high purity, all indexes meet the requirements of optical glass and laser glass raw materials, and a key high-purity raw material is provided for the industrial production of the laser glass and the civil optical glass.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive labor.
Fig. 1 is a flow chart of a method for preparing optical grade calcium metaphosphate according to the technical scheme of the invention.
Detailed Description
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
As shown in fig. 1, the preparation method of optical grade calcium metaphosphate in the present invention comprises the following steps:
1) reacting a calcium source (illustrated in figure 1 by taking industrial calcium hydroxide as an example) with industrial phosphoric acid and water according to a certain proportion under the conditions of heating and pressurizing to obtain a crude calcium dihydrogen phosphate solution;
2) adjusting the concentration of the crude calcium dihydrogen phosphate solution and enabling the crude calcium dihydrogen phosphate solution to pass through ion exchange resin to remove nonferrous metals and impurity ions;
3) evaporating and concentrating the solution after ion exchange resin, and concentrating to more than 25%;
4) carrying out first clean calcination to remove free water and structural water to obtain calcium metaphosphate intermediate powder;
5) and carrying out secondary clean calcination to obtain the optical grade calcium metaphosphate finished product.
Example 1
The preparation method of the optical grade calcium metaphosphate comprises the following steps:
1) adding 100kg of 98 percent calcium hydroxide into dilute phosphoric acid blended by 307.6kg of 85 percent industrial phosphoric acid and 738.4kg of water for reaction, controlling the reaction temperature to be 125-128 ℃, the reaction pressure to be 0.3-0.34 MPa, and the reaction time to be 5-6 h to obtain a crude calcium dihydrogen phosphate solution;
2) adjusting the concentration of the crude calcium dihydrogen phosphate solution to 11%, passing through ion exchange resin at a flow rate of 4.5L/min to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni, Co, etc. and Cl-Ion exchange resin comprises cation exchange resin of D402, D405 and IONRESIN 1600 type and anion exchange resin of D201 and D407 type;
3) evaporating and concentrating the solution after passing through the ion exchange resin to 26%;
4) after concentration, calcium dihydrogen phosphate solution enters a spray calcining tower through an industrial peristaltic pump at the flow rate of 10L/min for first clean calcination to remove free water and structural water, the air inlet temperature of the calcining tower is controlled to be 750-770 ℃, the temperature of the upper section of the tower body is controlled to be 720-740 ℃, the temperature of the middle section of the tower body is 685-705 ℃, the temperature of the lower section of the tower body is controlled to be 650-670 ℃, and the air outlet temperature is controlled to be 415-430 ℃ to obtain 269kg of calcium metaphosphate intermediate powder;
5) and (3) carrying out secondary clean calcination on the calcium metaphosphate intermediate powder in an electric furnace lined with the high-purity corundum material, wherein the calcination temperature is 820 ℃, and the calcination time is 5 hours, so that 252kg of optical-grade calcium metaphosphate finished products are obtained, and the comprehensive yield is 95.9%.
Example 2
The preparation method of the optical grade calcium metaphosphate comprises the following steps:
1) adding 110kg of 97 percent calcium hydroxide into 334.1kg of 85 percent industrial phosphoric acid and 801.9kg of diluted phosphoric acid blended by water to react, controlling the reaction temperature to be 128-132 ℃, the reaction pressure to be 0.34-0.37 MPa, and the reaction time to be 4-5 h to obtain a crude calcium dihydrogen phosphate solution;
2) adjusting the concentration of the crude calcium dihydrogen phosphate solution to 12%, passing through ion exchange resin at a flow rate of 4.2L/min to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni, Co, etc. and Cl-And sulfate radical, wherein the ion exchange resin is composed of cation exchange resin of D401 and D402 types and anion exchange resin of 201 × 7, D201 and D202 types;
3) evaporating and concentrating the solution after passing through the ion exchange resin to 26%;
4) after concentration, the calcium dihydrogen phosphate solution enters a spray calcining tower through an industrial peristaltic pump at the flow rate of 11L/min for first clean calcination to remove free water and structural water, the air inlet temperature of the calcining tower is controlled to be 760-780 ℃, the temperature of the upper section of the tower body is controlled to be 730-750 ℃, the temperature of the middle section of the tower body is controlled to be 700-720 ℃, the temperature of the lower section of the tower body is controlled to be 665-685 ℃, and the air outlet temperature is controlled to be 425-445 ℃ to obtain 291kg of calcium metaphosphate intermediate powder;
5) and (3) carrying out secondary clean calcination on the calcium metaphosphate intermediate powder in an electric furnace lined with a high-purity corundum material at 825 ℃ for 5h to obtain 275kg of optical-grade calcium metaphosphate finished products, wherein the comprehensive yield is 96.3%.
Example 3
The preparation method of the optical grade calcium metaphosphate comprises the following steps:
1) adding 112kg of 98 percent calcium hydroxide into dilute phosphoric acid blended by 344.7kg of 85 percent industrial phosphoric acid and 827.3kg of water for reaction, controlling the reaction temperature to be 130-134 ℃, the reaction pressure to be 0.37-0.42 MPa, and the reaction time to be 4-5 h to obtain a crude calcium dihydrogen phosphate solution;
2) adjusting the concentration of the crude calcium dihydrogen phosphate solution to 13%, and passing through ion exchange resin at a flow rate of 4L/min to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni, Co, etc. and Cl-Ion exchange resin comprises 732, D401 and IONRESIN35 type cation exchange resin and 201 × 7, D202 and IONRESIN IRA400 type anion exchange resin;
3) evaporating and concentrating the solution after ion exchange resin, and concentrating to 28%;
4) after concentration, calcium dihydrogen phosphate solution enters a spray calcining tower through an industrial peristaltic pump at the flow rate of 10.5L/min for first clean calcination to remove free water and structural water, the air inlet temperature of the calcining tower is controlled to be 755-770 ℃, the temperature of the upper section of the tower body is controlled to be 725-740 ℃, the temperature of the middle section of the tower body is controlled to be 692-705 ℃, the temperature of the lower section of the tower body is controlled to be 663-670 ℃, the air outlet temperature is controlled to be 421-430 ℃ and 303kg of calcium metaphosphate intermediate powder is obtained;
5) and (3) carrying out secondary clean calcination on the calcium metaphosphate intermediate powder in an electric furnace lined with a high-purity corundum material at the calcination temperature of 830 ℃ for 5 hours to obtain 285kg of optical-grade calcium metaphosphate finished product, wherein the comprehensive yield is 96.8%.
Example 4
The preparation method of the optical grade calcium metaphosphate comprises the following steps:
1) adding 125kg of 96.5 percent calcium hydroxide into 378.5kg of 85 percent industrial phosphoric acid and 908.5kg of diluted phosphoric acid blended by water to react, controlling the reaction temperature to be 134-138 ℃, the reaction pressure to be 0.41-0.46 MPa, and the reaction time to be 4-4.5 h to obtain a crude calcium dihydrogen phosphate solution;
2) adjusting the concentration of the crude calcium dihydrogen phosphate solution to 10%, passing through ion exchange resin at a flow rate of 4.8L/min to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni, Co, etc. and Cl-Ion exchange resin comprises 732 type cation exchange resin and IONRESIN 1600 type cation exchange resin, and 201 × 7 type anion exchange resin, D202 type anion exchange resin and D407 type anion exchange resin;
3) evaporating and concentrating the solution after ion exchange resin to 29%;
4) after concentration, calcium dihydrogen phosphate solution enters a spray calcining tower through an industrial peristaltic pump at the flow rate of 9.5L/min for first clean calcination to remove free water and structural water, the air inlet temperature of the calcining tower is controlled to be 750-765 ℃, the temperature of the upper section of the tower body is controlled to be 720-735 ℃, the temperature of the middle section of the tower body is 685-700 ℃, the temperature of the lower section of the tower body is controlled to be 650-665 ℃, the air outlet temperature is 415-426 ℃ to obtain 347kg of calcium metaphosphate intermediate powder;
5) and (3) carrying out secondary clean calcination on the calcium metaphosphate intermediate powder in an electric furnace lined with the high-purity corundum material at 835 ℃ for 5 hours to obtain 328kg of optical-grade calcium metaphosphate finished product with the comprehensive yield of 96.1%.
The calcium metaphosphate samples prepared in examples 1 to 4 were analyzed, and the results are shown in table 1:
TABLE 1 analysis of calcium metaphosphate samples
As can be seen from Table 1, in the calcium metaphosphate prepared in examples 1 to 4, Fe2O3The total content of 10 key impurity indexes of Cu, Co, Cr, Mn, Ni, Pb and the like does not exceed 5ppm, wherein the total content of Co, Cr, Mn, Ni, Pb and the likeThe total content is not more than 1ppm, Cu content is not more than 0.2ppm, Fe2O3Content of not more than 2ppm, Cl-The total content of sulfate radicals is not more than 150ppm, the content of CaO is 28 +/-0.5 percent, and P2O5The content is 72 +/-0.5%.
In conclusion, the optical calcium metaphosphate prepared by the method has high main content, low impurity content, stable quality and uniform granularity, all indexes meet the index requirements of raw materials of laser glass and optical glass, and the preparation method of the optical calcium metaphosphate is efficient, simple and convenient and has low production cost.
While specific embodiments of the present invention have been described in detail above, it will be appreciated that those skilled in the art, upon attaining an understanding of the foregoing may readily produce alterations to, variations of, and equivalents to these embodiments. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (9)
1. A preparation method of optical-grade calcium metaphosphate is characterized by comprising the following steps:
1) reacting a calcium source with phosphoric acid and water according to a certain proportion under the conditions of heating and pressurizing to obtain a crude calcium dihydrogen phosphate solution, wherein the calcium source is selected from calcium hydroxide or calcium oxide;
2) adjusting the concentration of the crude calcium dihydrogen phosphate solution and enabling the crude calcium dihydrogen phosphate solution to pass through ion exchange resin to remove nonferrous metals and impurity ions;
3) evaporating and concentrating the solution after ion exchange resin, and concentrating to more than 25%;
4) carrying out first clean calcination to remove free water and structural water to obtain calcium metaphosphate intermediate powder;
5) and carrying out secondary clean calcination to obtain the optical grade calcium metaphosphate finished product.
2. The method for preparing optical grade calcium metaphosphate according to claim 1, wherein the molar ratio of said calcium source to said phosphoric acid is 1 (1.97-2.03), and the mass ratio of said phosphoric acid to water is 1 (2.1-3.5).
3. The process for preparing optical grade calcium metaphosphate according to claim 1, wherein in step 1), the reaction temperature is 120-140 ℃, the reaction pressure is 0.25-0.5 MPa, and the reaction time is 3-7 h.
4. The method of claim 1, wherein the concentration of the crude monocalcium phosphate solution is adjusted to 8% to 16%.
5. The method of claim 1, wherein the flow rate of the crude monocalcium phosphate solution through the ion exchange resin is from 1L/min to 5L/min.
6. The method of claim 1, wherein the ion exchange resin comprises a cation exchange resin and an anion exchange resin, the cation exchange resin comprises one or more of 732, D401, D402, D405, IONRISI 1600 and IONRISI 35, and the anion exchange resin comprises one or more of 201 × 7, D201, D202, D407 and IONRISI IRA 400.
7. The process for preparing optical grade calcium metaphosphate according to claim 1, wherein in step 3), the concentration is 25% to 30%.
8. The method for preparing optical grade calcium metaphosphate according to claim 1, wherein the concentrated calcium dihydrogen phosphate solution enters the spray calcination tower at a flow rate of 5L/min to 13L/min for the first clean calcination, wherein the inlet air temperature is 720 ℃ to 800 ℃, the upper section temperature of the tower body is 690 ℃ to 770 ℃, the middle section temperature of the tower body is 660 ℃ to 740 ℃, the lower section temperature of the tower body is 630 ℃ to 705 ℃, and the outlet air temperature is 400 ℃ to 475 ℃.
9. The method for preparing optical grade calcium metaphosphate according to claim 1, wherein the second clean calcination is carried out in an electric furnace, the calcination temperature of the electric furnace is 760 ℃ to 860 ℃, and the calcination time is 4h to 10 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010415023.4A CN111422849A (en) | 2020-05-15 | 2020-05-15 | Preparation method of optical-grade calcium metaphosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010415023.4A CN111422849A (en) | 2020-05-15 | 2020-05-15 | Preparation method of optical-grade calcium metaphosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111422849A true CN111422849A (en) | 2020-07-17 |
Family
ID=71558810
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010415023.4A Pending CN111422849A (en) | 2020-05-15 | 2020-05-15 | Preparation method of optical-grade calcium metaphosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111422849A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114408890A (en) * | 2022-03-14 | 2022-04-29 | 上海太洋科技有限公司 | Method for preparing optical calcium metaphosphate from phosphorus-containing waste liquid |
| CN114852984A (en) * | 2022-05-30 | 2022-08-05 | 上海太洋科技有限公司 | Preparation method of optical-grade lithium metaphosphate |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU179284A (en) * | ||||
| CN1090255A (en) * | 1993-01-13 | 1994-08-03 | 北京市营养源研究所 | The preparation method of Trisodium trimetaphosphate |
| CN1761616A (en) * | 2003-03-14 | 2006-04-19 | 日本化学工业株式会社 | High purity metaphosphate and method for production thereof |
| CN1800001A (en) * | 2004-12-31 | 2006-07-12 | 西安交通大学医学院 | Calcium metaphosphorate production process |
| CN102311107A (en) * | 2011-08-30 | 2012-01-11 | 四川明晶光电科技有限公司 | Preparation method for colorless glass-state electronic-grade magnesium metaphosphate |
| CN102408103A (en) * | 2011-08-30 | 2012-04-11 | 四川明晶光电科技有限公司 | Temperature control stepwise conversion method of producing electronic grade aluminum metaphosphate |
-
2020
- 2020-05-15 CN CN202010415023.4A patent/CN111422849A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU179284A (en) * | ||||
| CN1090255A (en) * | 1993-01-13 | 1994-08-03 | 北京市营养源研究所 | The preparation method of Trisodium trimetaphosphate |
| CN1761616A (en) * | 2003-03-14 | 2006-04-19 | 日本化学工业株式会社 | High purity metaphosphate and method for production thereof |
| CN1800001A (en) * | 2004-12-31 | 2006-07-12 | 西安交通大学医学院 | Calcium metaphosphorate production process |
| CN102311107A (en) * | 2011-08-30 | 2012-01-11 | 四川明晶光电科技有限公司 | Preparation method for colorless glass-state electronic-grade magnesium metaphosphate |
| CN102408103A (en) * | 2011-08-30 | 2012-04-11 | 四川明晶光电科技有限公司 | Temperature control stepwise conversion method of producing electronic grade aluminum metaphosphate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114408890A (en) * | 2022-03-14 | 2022-04-29 | 上海太洋科技有限公司 | Method for preparing optical calcium metaphosphate from phosphorus-containing waste liquid |
| CN114408890B (en) * | 2022-03-14 | 2023-08-04 | 上海太洋科技有限公司 | Method for preparing optical grade calcium metaphosphate from phosphorus-containing waste liquid |
| CN114852984A (en) * | 2022-05-30 | 2022-08-05 | 上海太洋科技有限公司 | Preparation method of optical-grade lithium metaphosphate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111362244A (en) | Preparation method of optical-grade barium metaphosphate | |
| CN111422849A (en) | Preparation method of optical-grade calcium metaphosphate | |
| CN109775678A (en) | The method that battery-grade iron phosphate and PHOSPHORIC ACID TECH.GRADE lithium are prepared in waste lithium iron phosphate battery | |
| CN107337203B (en) | Method for preparing high-purity graphite | |
| CN109704408A (en) | A kind of production method of LITHIUM BATTERY high purity manganese sulfate | |
| CN108946694A (en) | A kind of hydrothermal synthesis method of battery-grade iron phosphate | |
| CN106169580B (en) | A kind of preparation method of battery-grade iron phosphate/graphene composite material | |
| CN105036159A (en) | Method for preparing lithium carbonate with high-lithium salt lake bittern | |
| CN109809440B (en) | Method for preparing high-purity lithium chloride, high-purity lithium formate and high-purity lithium carbonate | |
| CN106800283B (en) | Production method of powdery fire-fighting grade monoammonium phosphate | |
| CN111392704A (en) | Preparation method of optical-grade aluminum metaphosphate | |
| CN111348635A (en) | Preparation method of optical-grade potassium metaphosphate | |
| CN112645396B (en) | Method for treating fluorine-containing nickel slag generated in nitrogen trifluoride preparation process | |
| CN104495949B (en) | A kind of method utilizing titanium white waste acid to produce red iron oxide and manganous carbonate | |
| CN113772646A (en) | Wet-process phosphoric acid two-stage membrane deep purification process | |
| CN113184927A (en) | Method for producing nickel sulfate solution by using nickel powder | |
| CN108341421B (en) | Method for directly preparing lithium carbonate from salt lake brine with high magnesium-lithium ratio | |
| CN111483993A (en) | Preparation method of optical-grade lithium metaphosphate | |
| CN111087006B (en) | Novel preparation process for co-production of refined liquid salt and anhydrous sodium sulfate for alkali preparation | |
| CN111302321A (en) | Preparation method of optical-grade sodium metaphosphate | |
| CN101920994A (en) | Method for preparing vanadyl sulfate | |
| CN108793201B (en) | Method for purifying lithium chloride conversion solution | |
| CN1365948A (en) | Process for preparing industrial beryllium oxide by sulfuric acid method | |
| CN111422848A (en) | Preparation method of optical-grade zinc metaphosphate | |
| CN110407241B (en) | Preparation method of high-activity calcium oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200717 |
|
| RJ01 | Rejection of invention patent application after publication |