CN102408103B - Temperature control stepwise conversion method of producing electronic grade aluminum metaphosphate - Google Patents
Temperature control stepwise conversion method of producing electronic grade aluminum metaphosphate Download PDFInfo
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- CN102408103B CN102408103B CN2011102529872A CN201110252987A CN102408103B CN 102408103 B CN102408103 B CN 102408103B CN 2011102529872 A CN2011102529872 A CN 2011102529872A CN 201110252987 A CN201110252987 A CN 201110252987A CN 102408103 B CN102408103 B CN 102408103B
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Abstract
The invention discloses a temperature control stepwise conversion method of producing electronic grade aluminum metaphosphate, which comprises the following steps of: adding water and phosphoric acid in the weight ratio of 1 : 1 to a reaction kettle; slowly adding aluminum hydroxide after reacting completely,, and controlling the weight ratio of the added aluminum oxide to the phosphoric acid to 1 : 2; placing the produced aluminum dihydrogen phosphate in a box, and placing in a heating furnace, then closing the heating furnace; increasing temperature of the heating furnace, and extracting air to result in negative pressure state in the heating furnace; and carrying out temperature control baking to the heating furnace by three steps to obtain high-purity aluminum metaphosphate, taking out and cooling at room temperature. Using the method of carrying out stepwise conversion to the aluminum dihydrogen phosphate by controlling different temperatures to obtain the high-purity electronic grade aluminum metaphosphate, the characteristics of simple and clear operation steps, high stability and safety of industrial flow operation, high purity of produced aluminum metaphosphate, low production cost and batch production and the like can be realized.
Description
Technical field
The present invention relates to a kind of temperature control substep method for transformation of producing the electronic-grade aluminium metaphosphate.
Background technology
The utilization of aluminium metaphosphate in industry very extensively; Main as special optical glass; Phosphate glass, fluorphosphate glass and laser ignited glass additive etc., aluminium metaphosphate are better and specific refractory power is lower than other metaphosphate moisture resistivities in fluorphosphate glass, and Abbe number is also bigger; Thereby making that the ultraviolet portion chromatic dispersion of glass is lower, chemicalstability and physical strength are all fine.
Like patent 200710108995; A kind of method of manufacture of high purity aluminium metaphosphate; Each metal concentration of impurity is below 5ppm in the said high purity aluminium metaphosphate; This metal is at least a in iron, chromium, nickel, manganese or the copper, with aluminum oxide, white lake or phosphagel phosphaljel, puts into the sintering container that is covered with the aluminium metaphosphate powder in advance with phosphoric anhydride and Tripyrophosphoric acid mixing gained mixture and carries out sintering.The prepared aluminium metaphosphate purity of this patent is not high enough; Contain metallic impurity such as iron, chromium, nickel, manganese and copper; Adopt aluminum oxide, white lake or phosphagel phosphaljel to mix with phosphoric anhydride and Tripyrophosphoric acid, the starting material of manipulation require are more, cost is high and security and poor stability.
In general, there is following problem in existing aluminium metaphosphate preparation method: (1) complex operation step, and industrial flow processing safety, stability are all relatively poor, and easy error; (2) the aluminium metaphosphate purity of producing is not high enough, has directly influenced the quality of special optical glass; (3) production cost is high; (4) be difficult to realize mass production.
Summary of the invention
The objective of the invention is to solve existing deficiency of producing the method for aluminium metaphosphate; A kind of temperature control substep method for transformation of novel production electronic-grade aluminium metaphosphate is provided; Overcome the conventional production methods complex operation step; Industrial flow processing safety difference and easy error, the aluminium metaphosphate purity of producing is not high enough, and production cost is high and be difficult to realize shortcoming such as mass production.
The objective of the invention is to realize through following technical scheme: a kind of temperature control substep method for transformation of producing the electronic-grade aluminium metaphosphate, it may further comprise the steps:
(1) in reaction kettle, adding weight ratio is water and the phosphoric acid of 1:1;
(2) question response slowly adds white lake in the back fully in reaction kettle, and the weight ratio of the phosphoric acid that adds in the white lake amount of adding and the step (1) is 1:2;
(3) back that reacts completely generates aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate that generates is packed in the box, and place process furnace, sealed heating furnace;
(4) process furnace is warming up to 80 ~ 120 ℃, from process furnace, bleeds, make to be negative pressure state in the process furnace, air pressure is less than 1mmHg;
(5) process furnace is warming up to 280 ~ 320 ℃ and keep constant temperature calcining, roasting time 2.5 ~ 3.5 hours;
(6) process furnace behind step (5) constant temperature calcining is continued to be warming up to 480 ~ 520 ℃ and keep constant temperature calcining, roasting time 0.5 ~ 1.5 hour;
(7) process furnace behind step (6) constant temperature calcining is continued to be warming up to 880 ~ 920 ℃ and keep constant temperature calcining, roasting time 1.5 ~ 2.5 hours;
(8) aluminium metaphosphate that generates after the roasting is taken out from process furnace, and place the room temperature cooling.
The invention has the beneficial effects as follows: adopt the control different temperature that aluminium dihydrogen phosphate is carried out substep and transform and process high purity electronic-grade aluminium metaphosphate, have that operation steps is simple and clear, industrial flow operational stability and safe, the aluminium metaphosphate purity height produced, production cost is low and can realize characteristics such as mass production.
Embodiment
Further describe technical scheme of the present invention below in conjunction with specific embodiment:
[embodiment 1] a kind of temperature control substep method for transformation of producing the electronic-grade aluminium metaphosphate, it may further comprise the steps:
(1) in reaction kettle, adding weight ratio is water and the phosphoric acid of 1:1;
(2) question response slowly adds white lake in the back fully in reaction kettle, and the weight ratio of the phosphoric acid that adds in the white lake amount of adding and the step (1) is 1:2;
(3) back that reacts completely generates aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate that generates is packed in the box, and place process furnace, sealed heating furnace;
(4) process furnace is warming up to 80 ℃, from process furnace, bleeds, make to be negative pressure state in the process furnace, air pressure is less than 1mmHg;
(5) process furnace is warming up to 280 ℃ and keep constant temperature calcining, roasting time 2.5 hours;
(6) process furnace behind step (5) constant temperature calcining is continued to be warming up to 480 ℃ and keep constant temperature calcining, roasting time 0.5 hour;
(7) process furnace behind step (6) constant temperature calcining is continued to be warming up to 880 ℃ and keep constant temperature calcining, roasting time 1.5 hours;
(8) aluminium metaphosphate that generates after the roasting is taken out from process furnace, and place the room temperature cooling.
[embodiment 2] a kind of temperature control substep method for transformation of producing the electronic-grade aluminium metaphosphate, it may further comprise the steps:
(1) in reaction kettle, adding weight ratio is water and the phosphoric acid of 1:1;
(2) question response slowly adds white lake in the back fully in reaction kettle, and the weight ratio of the phosphoric acid that adds in the white lake amount of adding and the step (1) is 1:2;
(3) back that reacts completely generates aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate that generates is packed in the box, and place process furnace, sealed heating furnace;
(4) process furnace is warming up to 120 ℃, from process furnace, bleeds, make to be negative pressure state in the process furnace, air pressure is less than 1mmHg;
(5) process furnace is warming up to 320 ℃ and keep constant temperature calcining, roasting time 3.5 hours;
(6) process furnace behind step (5) constant temperature calcining is continued to be warming up to 520 ℃ and keep constant temperature calcining, roasting time 1.5 hours;
(7) process furnace behind step (6) constant temperature calcining is continued to be warming up to 920 ℃ and keep constant temperature calcining, roasting time 2.5 hours;
(8) aluminium metaphosphate that generates after the roasting is taken out from process furnace, and place the room temperature cooling.
[embodiment 3] a kind of temperature control substep method for transformation of producing the electronic-grade aluminium metaphosphate, it may further comprise the steps:
(1) in reaction kettle, adding weight ratio is water and the phosphoric acid of 1:1;
(2) question response slowly adds white lake in the back fully in reaction kettle, and the weight ratio of the phosphoric acid that adds in the white lake amount of adding and the step (1) is 1:2;
(3) back that reacts completely generates aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate that generates is packed in the box, and place process furnace, sealed heating furnace;
(4) process furnace is warming up to 100 ℃, from process furnace, bleeds, make to be negative pressure state in the process furnace, air pressure is less than 1mmHg;
(5) process furnace is warming up to 300 ℃ and keep constant temperature calcining, roasting time 3 hours;
(6) process furnace behind step (5) constant temperature calcining is continued to be warming up to 500 ℃ and keep constant temperature calcining, roasting time 1 hour;
(7) process furnace behind step (6) constant temperature calcining is continued to be warming up to 900 ℃ and keep constant temperature calcining, roasting time 2 hours;
(8) aluminium metaphosphate that generates after the roasting is taken out from process furnace, and place the room temperature cooling.
[embodiment 4] a kind of temperature control substep method for transformation of producing the electronic-grade aluminium metaphosphate, it may further comprise the steps:
(1) in reaction kettle, adding weight ratio is water and the phosphoric acid of 1:1;
(2) question response slowly adds white lake in the back fully in reaction kettle, and the weight ratio of the phosphoric acid that adds in the white lake amount of adding and the step (1) is 1:2;
(3) back that reacts completely generates aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate that generates is packed in the box, and place process furnace, sealed heating furnace;
(4) process furnace is warming up to 80 ℃, from process furnace, bleeds, make to be negative pressure state in the process furnace, air pressure is less than 1mmHg;
(5) process furnace is warming up to 280 ℃ and keep constant temperature calcining, roasting time 3.5 hours;
(6) process furnace behind step (5) constant temperature calcining is continued to be warming up to 480 ℃ and keep constant temperature calcining, roasting time 1.5 hours;
(7) process furnace behind step (6) constant temperature calcining is continued to be warming up to 880 ℃ and keep constant temperature calcining, roasting time 2.5 hours;
(8) aluminium metaphosphate that generates after the roasting is taken out from process furnace, and place the room temperature cooling.
[embodiment 5] a kind of temperature control substep method for transformation of producing the electronic-grade aluminium metaphosphate, it may further comprise the steps:
(1) in reaction kettle, adding weight ratio is water and the phosphoric acid of 1:1;
(2) question response slowly adds white lake in the back fully in reaction kettle, and the weight ratio of the phosphoric acid that adds in the white lake amount of adding and the step (1) is 1:2;
(3) back that reacts completely generates aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate that generates is packed in the box, and place process furnace, sealed heating furnace;
(4) process furnace is warming up to 100 ℃, from process furnace, bleeds, make to be negative pressure state in the process furnace, air pressure is less than 1mmHg;
(5) process furnace is warming up to 320 ℃ and keep constant temperature calcining, roasting time 2.5 hours;
(6) process furnace behind step (5) constant temperature calcining is continued to be warming up to 480 ℃ and keep constant temperature calcining, roasting time 1.5 hours;
(7) process furnace behind step (6) constant temperature calcining is continued to be warming up to 880 ℃ and keep constant temperature calcining, roasting time 2.5 hours;
(8) aluminium metaphosphate that generates after the roasting is taken out from process furnace, and place the room temperature cooling.
Claims (1)
1. temperature control substep method for transformation of producing the electronic-grade aluminium metaphosphate, it is characterized in that: it may further comprise the steps:
(1) in reaction kettle, adding weight ratio is water and the phosphoric acid of 1:1;
(2) question response slowly adds white lake in the back fully in reaction kettle, and the weight ratio of the phosphoric acid that adds in the white lake amount of adding and the step (1) is 1:2;
(3) back that reacts completely generates aluminium dihydrogen phosphate, the aluminium dihydrogen phosphate that generates is packed in the box, and place process furnace, sealed heating furnace;
(4) process furnace is warming up to 80 ~ 120 ℃, from process furnace, bleeds, make to be negative pressure state in the process furnace, air pressure is less than 1mmHg;
(5) process furnace is warming up to 280 ~ 320 ℃ and keep constant temperature calcining, roasting time 2.5 ~ 3.5 hours;
(6) process furnace behind step (5) constant temperature calcining is continued to be warming up to 480 ~ 520 ℃ and keep constant temperature calcining, roasting time 0.5 ~ 1.5 hour;
(7) process furnace behind step (6) constant temperature calcining is continued to be warming up to 880 ~ 920 ℃ and keep constant temperature calcining, roasting time 1.5 ~ 2.5 hours;
(8) aluminium metaphosphate that generates after the roasting is taken out from process furnace, and place the room temperature cooling.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107500261B (en) * | 2017-08-23 | 2019-12-24 | 广西新晶科技有限公司 | Aluminum metaphosphate powder for optical glass and preparation method thereof |
| CN110116998A (en) * | 2018-02-05 | 2019-08-13 | 江苏省国盛稀土有限公司 | A kind of preparation method of high-purity aluminium metaphosphate powder |
| CN110092364B (en) * | 2019-05-13 | 2021-08-20 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity optical glass additive zinc metaphosphate |
| CN110040708B (en) * | 2019-05-13 | 2020-09-25 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity optical glass additive lanthanum metaphosphate |
| CN110054166B (en) * | 2019-05-13 | 2020-09-25 | 承德莹科精细化工股份有限公司 | Preparation method of high-purity ytterbium metaphosphate as optical glass additive |
| CN111392704A (en) * | 2020-04-10 | 2020-07-10 | 上海太洋科技有限公司 | Preparation method of optical-grade aluminum metaphosphate |
| CN111422849A (en) * | 2020-05-15 | 2020-07-17 | 上海太洋科技有限公司 | Preparation method of optical-grade calcium metaphosphate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4329327A (en) * | 1980-11-26 | 1982-05-11 | Ppg Industries, Inc. | Method for making B-form aluminum trimetaphosphate from powder reactants |
| CN101037194A (en) * | 2003-03-14 | 2007-09-19 | 日本化学工业株式会社 | High purity metaphosphate and its production method |
| CN101172596A (en) * | 2007-10-10 | 2008-05-07 | 广西民族大学 | Method for rapid synthesis of aluminum orthophosphate salt polyalcohol |
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- 2011-08-30 CN CN2011102529872A patent/CN102408103B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4329327A (en) * | 1980-11-26 | 1982-05-11 | Ppg Industries, Inc. | Method for making B-form aluminum trimetaphosphate from powder reactants |
| CN101037194A (en) * | 2003-03-14 | 2007-09-19 | 日本化学工业株式会社 | High purity metaphosphate and its production method |
| CN101172596A (en) * | 2007-10-10 | 2008-05-07 | 广西民族大学 | Method for rapid synthesis of aluminum orthophosphate salt polyalcohol |
Non-Patent Citations (2)
| Title |
|---|
| 三聚磷酸二氢铝二水物的合成工艺;袁爱群;《四川化工与腐蚀控制》;20001231;第3卷(第3期);9-12 * |
| 袁爱群.三聚磷酸二氢铝二水物的合成工艺.《四川化工与腐蚀控制》.2000,第3卷(第3期),9-12. |
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