CN111392704A - Preparation method of optical-grade aluminum metaphosphate - Google Patents
Preparation method of optical-grade aluminum metaphosphate Download PDFInfo
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
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- C01B25/38—Condensed phosphates
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Abstract
The technical scheme of the invention provides a preparation method of optical-grade aluminum metaphosphate, which comprises the following steps: reacting aluminum hydroxide or aluminum oxide with phosphoric acid and water according to a certain proportion to obtain a crude aluminum dihydrogen phosphate solution; adjusting the concentration of the crude aluminum dihydrogen phosphate solution, and enabling the crude aluminum 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 40%; carrying out first clean calcination to remove free water and structural water to obtain aluminum metaphosphate intermediate powder; and carrying out secondary clean calcination to obtain the optical grade aluminum metaphosphate finished product. The preparation method of the technical scheme has strong adaptability to the raw materials of aluminum hydroxide or aluminum oxide, the aluminum metaphosphate prepared by removing impurities by an ion exchange method and combining indirect heating clean spray calcination with high-temperature electric furnace clean calcination has high purity, and all indexes meet the requirements of raw materials of optical glass and laser 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 aluminum 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.
Patent CN201810111408.4 discloses a method for obtaining high-purity aluminum metaphosphate by calcining high-purity aluminum phosphate powder obtained from an intermediate, namely hydrated aluminum phosphate, and an aluminum source (high-purity aluminum hydroxide) by means of hygroscopic weathering, wherein the method requires high-purity raw materials in the whole process, and has no chemical purification process, so that the method has significant material limitations, complicated operation steps, and the product purity is difficult to reach a relatively high degree (for example, the total amount of transition metal impurities is less than 2 ppm).
Disclosure of Invention
In view of the current state of the prior art, the technical problem to be solved by the invention is to provide a method for preparing optical-grade aluminum metaphosphate, wherein the main index of the prepared aluminum 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 aluminum metaphosphate, which comprises the following steps:
1) reacting aluminum hydroxide or aluminum oxide with phosphoric acid and water according to a certain proportion to obtain a crude aluminum dihydrogen phosphate solution;
2) adjusting the concentration of the crude aluminum dihydrogen phosphate solution, and enabling the crude aluminum 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 40%;
4) carrying out first clean calcination to remove free water and structural water to obtain aluminum metaphosphate intermediate powder;
5) and carrying out secondary clean calcination to obtain the optical grade aluminum metaphosphate finished product.
Preferably, in the step 1), the molar ratio of the aluminum hydroxide or the aluminum oxide to the phosphoric acid is 1 (5.9-6.1), the mass ratio of the phosphoric acid to the water is 1 (0.6-1.5), and the reaction temperature is 105-125 ℃. More preferably, the molar ratio of the aluminum hydroxide or the aluminum oxide to the phosphoric acid is 1 (5.95-6.05), the mass ratio of the phosphoric acid to the water is 1 (0.6-0.9), and the reaction temperature is 110-120 ℃.
Preferably, the concentration of the crude aluminum dihydrogen phosphate solution is adjusted to be 9 to 18 percent, and the flow rate passing through the ion exchange resin is 1L to 5L/min, further preferably, the concentration of the crude aluminum dihydrogen phosphate solution is adjusted to be 9 to 14 percent, and the flow rate passing through the ion exchange resin is 2L to 4L/min.
Preferably, the ion exchange resin comprises cation exchange resin and anion exchange resin, the cation exchange resin comprises one or more of D401, D402, D403, D405, IONRIESIN 35, IONRIESIN 1600 and IONRIESIN 252, and the anion exchange resin comprises one or more of IONRIESIN IRA400, IONRISI IRA402, IONRISI IRA900, IONRISI IRA456 and D407.
Preferably, in the step 3), the concentration is carried out to 40 to 50 percent. More preferably, the concentration is 42-47%.
Preferably, the concentrated aluminum dihydrogen phosphate solution enters a spray calcining tower at the flow rate of 6L-15L/min for first clean calcination, wherein the air inlet temperature is 700-800 ℃, the temperature of the upper section of the tower body is 680-750 ℃, the temperature of the middle section of the tower body is 650-720 ℃, the temperature of the lower section of the tower body is 620-700 ℃, and the air outlet temperature is 400-500 ℃.
Furthermore, the concentrated aluminum dihydrogen phosphate solution enters a spray calcining tower at the flow rate of 9L/min-12L/min for first clean calcination, wherein the air inlet temperature is 680-730 ℃, the upper section temperature of the tower body is 650-700 ℃, the middle section temperature of the tower body is 630-680 ℃, the lower section temperature of the tower body is 600-630 ℃, and the air outlet temperature is 380-430 ℃.
In the spray calcination process, in order to ensure that the 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 air inlet temperature of a spray calcination tower can only reach 780-800 ℃ at most (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 the aluminum metaphosphate, at most 98% of aluminum dihydrogen phosphate structural water can be removed, and higher lasting temperature and further calcination equipment are required to remove 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 750-850 ℃, and the calcination time is 4-10 h.
Furthermore, in the step e, the electric furnace calcination temperature is 780-840 ℃, and the calcination time is 6-9 h. The hearth is made of high-purity alumina or high-purity quartz material as a lining.
The preparation method of the optical grade aluminum metaphosphate provided by the technical scheme of the invention has the following beneficial effects: the adaptability to raw materials of aluminum hydroxide or aluminum oxide and phosphoric acid is strong, the mode of removing impurities by an ion exchange method, indirectly heating, cleaning, spraying and calcining and combining with cleaning and calcining by a high-temperature electric furnace is adopted, the total amount of transition metal impurities can be controlled to be below 2ppm, ultra-pure aluminum metaphosphate can be produced, and all indexes meet the requirements of raw materials of optical glass and laser 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 aluminum 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 aluminum metaphosphate in the technical scheme of the invention comprises the following steps:
1) reacting aluminum hydroxide or aluminum oxide with phosphoric acid and water according to a certain proportion (namely heating gradual reaction in figure 1) to obtain a crude aluminum dihydrogen phosphate solution;
2) adjusting the concentration of the crude aluminum dihydrogen phosphate solution, and enabling the crude aluminum 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 40%;
4) carrying out first clean calcination to remove free water and structural water to obtain aluminum metaphosphate intermediate powder;
5) and carrying out secondary clean calcination to obtain the optical grade aluminum metaphosphate finished product.
Example 1
The preparation method of the optical-grade aluminum metaphosphate comprises the following steps:
1) gradually adding 100kg of 97.5 percent alumina into dilute phosphoric acid blended by 664.1kg of 85 percent industrial phosphoric acid and 464.9kg of water, and controlling the reaction temperature to be 110-115 ℃ to obtain a crude aluminum dihydrogen phosphate solution;
2) adjusting the concentration of the crude aluminum dihydrogen phosphate solution to 12%, and passing through a group of composite ion exchange devices filled with D403, D405 and IONRESIN 35 type cation exchange resins and specially selected IONRESIN IRA402 and IONRESIN IRA900 type anion exchange resins at the flow rate of 4L/min to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni and Co and Cl－Sulfate radicals and the like;
3) evaporating and concentrating the solution after ion exchange resin, and concentrating to 45%;
4) controlling the concentrated aluminum dihydrogen phosphate solution by an industrial peristaltic pump, feeding the concentrated aluminum dihydrogen phosphate solution into a spray calcining tower at the flow rate of 10L/min, and controlling the air inlet temperature of the calcining tower to be 700-720 ℃, the upper section temperature of the tower body to be 660-690 ℃, the middle section temperature of the tower body to be 630-660 ℃, the lower section temperature of the tower body to be 600-620 ℃ and the air outlet temperature to be 390-420 ℃ to obtain 515kg aluminum metaphosphate intermediate powder;
5) calcining the intermediate powder of the aluminum metaphosphate in an electric furnace lined with a high-purity corundum material at 800 ℃ for 6 hours to obtain 492kg of optical-grade aluminum metaphosphate finished product with the comprehensive yield of 97.5 percent.
Example 2
The preparation method of the optical-grade aluminum metaphosphate comprises the following steps:
1)120kg of alumina with the content of 96 percent is gradually added into diluted phosphoric acid which is blended by 780kg of 85 percent industrial phosphoric acid and 546kg of water, the reaction temperature is controlled to be 110-115 ℃, and a crude aluminum dihydrogen phosphate solution is obtained;
2) adjusting the concentration of the crude aluminum dihydrogen phosphate solution to 10%, and passing through a group of composite ion exchange devices filled with aluminum salt modified D401 and D402 type cation exchange resins and specially selected IONRISI IRA456 and D407 type anion exchange resins at a flow rate of 5L/min to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni and Co and Cl－Sulfate radicals and the like;
3) evaporating and concentrating the solution after ion exchange resin, and concentrating to 42%;
4) controlling the concentrated aluminum dihydrogen phosphate solution by an industrial peristaltic pump, feeding the concentrated aluminum dihydrogen phosphate solution into a spray calcining tower at the flow rate of 12L/min, and controlling the air inlet temperature of the calcining tower to be 720-740 ℃, the upper section temperature of the tower body to be 670-690 ℃, the middle section temperature of the tower body to be 640-665 ℃, the lower section temperature of the tower body to be 610-625 ℃ and the air outlet temperature to be 400-420 ℃ to obtain 602kg of aluminum metaphosphate intermediate powder;
5) calcining the aluminum metaphosphate intermediate powder in an electric furnace lined with a high-purity corundum material at 820 ℃ for 5 hours to obtain optical grade aluminum metaphosphate finished product 572kg, wherein the comprehensive yield is 95.9%.
Example 3
The preparation method of the optical-grade aluminum metaphosphate comprises the following steps:
1)140kg of alumina with the content of 97 percent is gradually added into dilute phosphoric acid blended by 928.2kg of 85 percent industrial phosphoric acid and 649.8kg of water, the reaction temperature is controlled to be 112-116 ℃, and a crude aluminum dihydrogen phosphate solution is obtained;
2) adjusting the concentration of the crude aluminum dihydrogen phosphate solution to 11%, and passing through a group of composite ion exchange devices filled with aluminum salt modified D402, D403 and D405 type cation exchange resins and specially selected IONRISIN IRA400 and IONRISIRA 402 type anion exchange resins at the flow rate of 4.5L/min to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni and Co and Cl－Sulfate radicals and the like;
3) evaporating and concentrating the solution after ion exchange resin to 46%;
4) controlling the concentrated aluminum dihydrogen phosphate solution by an industrial peristaltic pump, feeding the concentrated aluminum dihydrogen phosphate solution into a spray calcining tower at the flow rate of 11L/min, and controlling the air inlet temperature of the calcining tower to be 720-750 ℃, the temperature of the upper section of the tower body to be 680-700 ℃, the temperature of the middle section of the tower body to be 650-670 ℃, the temperature of the lower section of the tower body to be 620-640 ℃ and the air outlet temperature to be 405-420 ℃ to obtain 710kg of aluminum metaphosphate intermediate powder;
5) calcining the intermediate powder of the aluminum metaphosphate in an electric furnace lined with a high-purity corundum material at 790 ℃ for 7 hours to obtain 668kg of optical grade aluminum metaphosphate finished product with the comprehensive yield of 95.1 percent.
Example 4
The preparation method of the optical-grade aluminum metaphosphate comprises the following steps:
1)200kg of alumina with the content of 96 percent is gradually added into dilute phosphoric acid which is blended by 1308.8kg of 85 percent industrial phosphoric acid and 916.2kg of water, the reaction temperature is controlled to be 110-115 ℃, and crude aluminum dihydrogen phosphate solution is obtained;
2) adjusting the concentration of the crude aluminum dihydrogen phosphate solution to 12%, and passing through a group of cation exchange resins filled with aluminum salt modified D405, IONRESIN 1600 and IONRESINIRA 252 and specially selected IONRESINIRA400, IONRESIN IRA402 and I at the flow rate of 4L/minComposite ion exchange device of ONRESIN IRA900 type anion exchange resin for removing Fe, Mn, Pb, Cr, Cu, Ni, Co and other nonferrous metals and Cl－Sulfate radicals and the like;
3) evaporating and concentrating the solution after ion exchange resin, and concentrating to 45%;
4) controlling the concentrated aluminum dihydrogen phosphate solution by an industrial peristaltic pump, feeding the concentrated aluminum dihydrogen phosphate solution into a spray calcining tower at the flow rate of 12L/min, controlling the air inlet temperature of the calcining tower to be 730-760 ℃, the upper section temperature of the tower body to be 690-720 ℃, the middle section temperature of the tower body to be 650-670 ℃, the lower section temperature of the tower body to be 615-630 ℃ and the air outlet temperature to be 400-420 ℃, and obtaining 989kg of aluminum metaphosphate intermediate powder;
5) calcining the aluminum metaphosphate intermediate powder in an electric furnace lined with a high-purity corundum material at 840 ℃ for 5 hours to obtain 949kg of optical grade aluminum metaphosphate finished product, wherein the comprehensive yield is 95.5%.
Example 5
The preparation method of the optical-grade aluminum metaphosphate comprises the following steps:
1)170kg of 98 percent alumina is gradually added into dilute phosphoric acid blended by 1127.6kg of 85 percent industrial phosphoric acid and 789.4kg of water, 1917kg of 50 percent industrial phosphoric acid, and the reaction temperature is controlled to be 113-118 ℃ to obtain a crude aluminum dihydrogen phosphate solution;
2) adjusting the concentration of the crude aluminum dihydrogen phosphate solution to 12.5%, and passing through a group of composite ion exchange devices filled with aluminum salt modified cation exchange resin IONRESIN 35 and IONRESIN 1600 type cation exchange resin and specially selected anion exchange resin IONRESIN IRA900 and IONRESIN IRA456 type anion exchange resin at the flow rate of 4.2L/min to remove nonferrous metals such as Fe, Mn, Pb, Cr, Cu, Ni and Co and Cl－Sulfate radicals and the like;
3) evaporating and concentrating the solution after ion exchange resin, and concentrating to 44%;
4) controlling the concentrated aluminum dihydrogen phosphate solution by an industrial peristaltic pump, feeding the concentrated aluminum dihydrogen phosphate solution into a spray calcining tower at the flow rate of 11L/min, and controlling the air inlet temperature of the calcining tower to be 740-770 ℃, the upper section temperature of the tower body to be 700-730 ℃, the middle section temperature of the tower body to be 660-680 ℃, the lower section temperature of the tower body to be 630-650 ℃ and the air outlet temperature to be 410-430 ℃ to obtain 854kg of aluminum metaphosphate intermediate powder;
5) calcining the intermediate powder of the aluminum metaphosphate in an electric furnace lined with a high-purity corundum material at 850 ℃ for 4.5 hours to obtain 827kg of optical grade aluminum metaphosphate finished products, wherein the comprehensive yield is 95.9%.
The aluminum metaphosphate samples prepared in examples 1 to 5 were analyzed, and the results are shown in table 1:
TABLE 1 analysis of samples of aluminum metaphosphate
As can be seen from Table 1, in the aluminum metaphosphate prepared in examples 1 to 5, Fe2O3The total content of 10 key impurities such as 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 like does not exceed 1ppm, the content of Cu does not exceed 0.2ppm, and Fe2O3Content of not more than 2ppm, Cl-The total content of sulfate radicals is not more than 100ppm, Al2O3Content 19 + -0.5%, P2O5The content is 81 plus or minus 0.5 percent.
In conclusion, the prepared optical-grade aluminum metaphosphate has the advantages of high main content, low impurity content, stable quality and uniform granularity, all indexes of the aluminum metaphosphate meet the index requirements of raw materials of laser glass and optical glass, and the preparation method of the optical-grade aluminum metaphosphate is efficient, simple and convenient and low in 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. The preparation method of optical-grade aluminum metaphosphate is characterized by comprising the following steps of:
1) reacting aluminum hydroxide or aluminum oxide with phosphoric acid and water according to a certain proportion to obtain a crude aluminum dihydrogen phosphate solution;
2) adjusting the concentration of the crude aluminum dihydrogen phosphate solution, and enabling the crude aluminum 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 40%;
4) carrying out first clean calcination to remove free water and structural water to obtain aluminum metaphosphate intermediate powder;
5) and carrying out secondary clean calcination to obtain the optical grade aluminum metaphosphate finished product.
2. The method for preparing optical grade aluminum metaphosphate according to claim 1, wherein in step 1), the molar ratio of aluminum hydroxide or aluminum oxide to the phosphoric acid is 1 (5.9-6.1), the mass ratio of phosphoric acid to water is 1 (0.6-1.5), and the reaction temperature is 105-125 ℃.
3. The method of claim 1, wherein the concentration of the crude aluminum dihydrogen phosphate solution is adjusted to 9% to 18% and the flow rate through the ion exchange resin is adjusted to 1L/min to 5L/min.
4. The method of claim 1, wherein the ion exchange resin comprises a cation exchange resin comprising one or a combination of D401, D402, D403, D405, iorreisin 35, iorreisin 1600, iorreisin 252, and an anion exchange resin comprising one or a combination of iorreisin IRA400, iorreisin IRA402, iorreisin IRA900, iorreisin IRA456, D407.
5. The method of claim 1, wherein the concentration in step 3) is between 40% and 50%.
6. The method for preparing optical grade aluminum metaphosphate as claimed in claim 1, wherein the concentrated aluminum dihydrogen phosphate solution enters the spray calcination tower at a flow rate of 6L/min-15L/min for the first clean calcination, wherein the inlet air temperature is 700 ℃ to 800 ℃, the upper section temperature of the tower body is 680 ℃ to 750 ℃, the middle section temperature of the tower body is 650 ℃ to 720 ℃, the lower section temperature of the tower body is 620 ℃ to 700 ℃, and the outlet air temperature is 400 ℃ to 500 ℃.
7. The method for preparing optical grade aluminum metaphosphate as in claim 6, wherein said spray-calcining tower is internally lined with high-purity alumina, the spray head is made of titanium-palladium alloy, and the heating method is indirect heating.
8. The method for preparing optical grade aluminum metaphosphate as set forth in claim 1, wherein the second clean calcination is carried out in an electric furnace, the calcination temperature of the electric furnace is 750-850 ℃, and the calcination time is 4-10 h.
9. The method of claim 8, wherein the hearth of the electric furnace is lined with a high purity alumina or high purity quartz material.
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| 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 |
| CN115028152A (en) * | 2022-05-12 | 2022-09-09 | 上海太洋科技有限公司 | Preparation method of optical-grade aluminum metaphosphate |
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