CN102862965A - Method of dissolving monopotassium phosphate powder - Google Patents
Method of dissolving monopotassium phosphate powder Download PDFInfo
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- CN102862965A CN102862965A CN2012103396923A CN201210339692A CN102862965A CN 102862965 A CN102862965 A CN 102862965A CN 2012103396923 A CN2012103396923 A CN 2012103396923A CN 201210339692 A CN201210339692 A CN 201210339692A CN 102862965 A CN102862965 A CN 102862965A
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Abstract
The invention discloses a method of dissolving monopotassium phosphate powder. The method comprises the following steps of: (1) adding ultra-pure water into a reaction kettle and heating the reaction kettle; (2) starting a stirring rod in the reaction kettle to stir; (3) when the temperature in the reaction kettle is 30-135 DEG C, feeding the monopotassium phosphate powder into the reaction kettle at the speed of 50-75 Kg/hour; (4) detecting the temperature in the reaction kettle, when the temperature in the reaction kettle is lower than 30 DEG C, stopping feeding the monopotassium phosphate powder into the reaction kettle, and when the temperature in the reaction kettle is 30-135 DEG C, feeding the monopotassium phosphate powder into the reaction kettle; and (5) repeatedly performing the step (4), when the mass ratio of the ultra-pure water to the monopotassium phosphate powder is 1: 0.5-0.7, stopping feeding the monopotassium phosphate powder into the reaction kettle, keeping the temperature in the reaction kettle to 30-135 DEG C, and stirring for 1-2 hours. According to the invention, the monopotassium phosphate powder is fully dissolved through heating and precisely controlling the heating temperature.
Description
Technical field
The present invention relates to a kind of dissolving method, particularly a kind of method of dissolving phosphoric acid potassium dihydrogen powder belongs to potassium primary phosphate purifying technology field.
Background technology
The KDP crystal is to make raw material with phosphoric acid salt, KDP does raw material with potassium primary phosphate to tuck in middle growth water-soluble, present large-sized KDP crystal is one of critical material of laser fusion, the KDP that uses in laser fusion requires to have high transmitance and high damage threshold, these index request crystal are highly pure, and this just needs highly pure raw material.
The purity of potassium primary phosphate is higher, the crystal of growth can be larger, when making eyeglass, just mean that also the eyeglass of doing can be larger, the light beam that can pass through within the unit time like this can be more, light beam is through after this crystal eyeglass, a cataclysm can occur, it can be heated up, be exactly traditional laser.
Therefore, the purity of potassium primary phosphate is extremely important.It is free metal ion with in the potassium primary phosphate that the powder of potassium dihydrogen phosphate crystal is purified, and comprises other impurity, effectively is controlled at below the 0.02ppm, makes its growth to crystal have controllability, makes crystal become pure and physical property is fixed.
The content of at present domestic potassium primary phosphate detrimental impurity there is no at present simple and reliable method potassium primary phosphate is purified below 10ppm.The purification water-soluble reagent is generally used the method for recrystallization, and utilize impurity in crystal and in the solvent difference of segregation coefficient reaches the purpose of purifying.
At first the potassium primary phosphate powder is dissolved in the ultrapure water in the recrystallization method, whether dissolving fully directly affects the follow-up work that potassium primary phosphate is purified.
Summary of the invention
Technical problem to be solved by this invention provides the method for in a kind of potassium primary phosphate purifying technique the potassium primary phosphate powder fully being dissolved.
In order to solve above-mentioned technical problem, technical scheme of the present invention is: a kind of method of dissolving phosphoric acid potassium dihydrogen powder may further comprise the steps:
(1) in reactor, adds ultrapure water and reactor heated;
(2) begin to start the interior agitator arm of reactor and stir, stirring velocity is 100-150 rev/min; Although do not drop into the potassium primary phosphate powder in this process, after the effect of stirring this moment is water flow, make the temperature of heating more even, efficient is high.
(3) when reactor temperature reaches 30-135 ℃, with 50-75Kg/ hour speed the potassium primary phosphate powder is dropped in the reactor; 30-135 ℃ of suitable potassium primary phosphate powder dissolving, best temperature is 115-135 ℃ certainly, preferred 115 ℃.
(4) because the potassium primary phosphate powder dissolves in ultrapure water after dropping into, and it is the process of a heat absorption that the potassium primary phosphate powder is dissolved in the water, and this process will be taken away certain heat, thereby cause the reactor internal temperature to descend.So just, be unfavorable for the dissolving of potassium primary phosphate powder in the subsequent process, therefore, answer the temperature of detection reaction still inside.When the reactor internal temperature is lower than 30 ℃, stop the potassium primary phosphate powder is dropped into reactor, when the reactor internal temperature reaches 30-135 ℃, continue the potassium primary phosphate powder is dropped in the reactor.The temperature of potassium primary phosphate powder dissolving just can accurately be grasped like this, promotes the abundant of dissolving.
(5) performing step (4) (namely only when the reactor internal temperature is 30-135 ℃, just the potassium primary phosphate powder being dropped in the reactor) repeatedly, when reaching 1:0.5-0.7, the mass ratio of ultrapure water and potassium primary phosphate powder stops in reactor, dropping into the potassium primary phosphate powder, keep reactor temperature at 30-135 ℃, and stirred 1-2 hour.Ultrapure water and the preferred mass ratio of potassium primary phosphate powder stop when being 1:0.625 dropping into the potassium primary phosphate powder in reactor.
Certainly, the mass ratio of potassium primary phosphate powder of the present invention and ultrapure water can be higher, and the present invention has taken into account efficient on the basis of considering solubleness, therefore given up higher mass ratio.
Described reactor is outside equipped with the spiral uprising shape heating tube, and reactor heats reactor by the thermal oil in the heating tube.
Temperature is very large for the dissolving impact of material, the present invention mainly reaches the purpose that potassium primary phosphate fully dissolves by the temperature of control potassium primary phosphate dissolving, make the potassium primary phosphate dissolving more abundant, has higher solubleness, the efficient of potassium primary phosphate powder dissolving is high, for good place mat is made in the follow-up work that potassium primary phosphate is purified.
Embodiment
Embodiment 1
At 1.5m
3Add the 1000kg ultrapure water in the reactor, reactor is outside equipped with the spiral uprising shape heating tube, and reactor heats reactor by the thermal oil in the heating tube, begins to start the interior agitator arm of reactor and stirs, and stirring velocity is 120 rev/mins.
When reactor temperature is heated to 35 ℃, with 50Kg/ hour speed the potassium primary phosphate powder is dropped in the reactor; By temperature sensor equitemperature proofing unit the reactor internal temperature is detected, when the reactor internal temperature is lower than 30 ℃, stop the potassium primary phosphate powder is dropped into reactor, when the reactor internal temperature reaches 35 ℃, continue the potassium primary phosphate powder is dropped in the reactor.
Performing step (4) repeatedly, when reaching 1:0.6, the mass ratio of ultrapure water and potassium primary phosphate powder stops in reactor, dropping into the potassium primary phosphate powder, keep reactor temperature at 30 ℃, and stirred 1.5 hours, the solubleness of potassium primary phosphate powder is 60 g/100 ml.
Embodiment 2
At 1.5m
3Add the 1000kg ultrapure water in the reactor, reactor is outside equipped with the spiral uprising shape heating tube, and reactor heats reactor by the thermal oil in the heating tube, begins to start the interior agitator arm of reactor and stirs, and stirring velocity is 150 rev/mins.
When reactor temperature is heated to 135 ℃, with 75Kg/ hour speed the potassium primary phosphate powder is dropped in the reactor; By temperature sensor equitemperature proofing unit the reactor internal temperature is detected, when the reactor internal temperature is lower than 30 ℃, stop the potassium primary phosphate powder is dropped into reactor, when the reactor internal temperature reaches 135 ℃, continue the potassium primary phosphate powder is dropped in the reactor.
Performing step (4) repeatedly, when reaching 1:0.7, the mass ratio of ultrapure water and potassium primary phosphate powder stops in reactor, dropping into the potassium primary phosphate powder, keep reactor temperature at 135 ℃, and stirred 2 hours, the solubleness of potassium primary phosphate powder is 70 g/100 ml.
Embodiment 3
At 1.5m
3Add the 1000kg ultrapure water in the reactor, reactor is outside equipped with the spiral uprising shape heating tube, and reactor heats reactor by the thermal oil in the heating tube, begins to start the interior agitator arm of reactor and stirs, and stirring velocity is 100 rev/mins.
When reactor temperature is heated to 115 ℃, with 62.5Kg/ hour speed the potassium primary phosphate powder is dropped in the reactor; By temperature sensor equitemperature proofing unit the reactor internal temperature is detected, when the reactor internal temperature is lower than 30 ℃, stop the potassium primary phosphate powder is dropped into reactor, when the reactor internal temperature reaches 115 ℃, continue the potassium primary phosphate powder is dropped in the reactor.
Performing step (4) repeatedly, when reaching 1:0.625, the mass ratio of ultrapure water and potassium primary phosphate powder stops in reactor, dropping into the potassium primary phosphate powder, keep reactor temperature at 115 ℃, and stirred 1 hour, the solubleness of potassium primary phosphate powder is 62.5 g/100 ml.
Embodiment 4
At 1.5m
3Add the 1000kg ultrapure water in the reactor, reactor is outside equipped with the spiral uprising shape heating tube, and reactor heats reactor by the thermal oil in the heating tube, begins to start the interior agitator arm of reactor and stirs, and stirring velocity is 135 rev/mins.
When reactor temperature is heated to 120 ℃, with 70Kg/ hour speed the potassium primary phosphate powder is dropped in the reactor; By temperature sensor equitemperature proofing unit the reactor internal temperature is detected, when the reactor internal temperature is lower than 30 ℃, stop the potassium primary phosphate powder is dropped into reactor, when the reactor internal temperature reaches 120 ℃, continue the potassium primary phosphate powder is dropped in the reactor.
Performing step (4) repeatedly, when reaching 1:0.65, the mass ratio of ultrapure water and potassium primary phosphate powder stops in reactor, dropping into the potassium primary phosphate powder, keep reactor temperature at 120 ℃, and stirred 1.5 hours, the solubleness of potassium primary phosphate powder is 65 g/100 ml.
Above-described embodiment does not limit the present invention in any way, and every employing is equal to replaces or technical scheme that the mode of equivalent transformation obtains all drops in protection scope of the present invention.
Claims (4)
1. the method for a dissolving phosphoric acid potassium dihydrogen powder is characterized in that may further comprise the steps:
(1) in reactor, adds ultrapure water and reactor heated;
(2) begin to start the interior agitator arm of reactor and stir, stirring velocity is 100-150 rev/min;
(3) when reactor temperature reaches 30-135 ℃, with 50-75Kg/ hour speed the potassium primary phosphate powder is dropped in the reactor;
(4) the reactor internal temperature is detected, when the reactor internal temperature is lower than 30 ℃, stop the potassium primary phosphate powder is dropped into reactor, when the reactor internal temperature reaches 30-135 ℃, continue the potassium primary phosphate powder is dropped in the reactor;
(5) performing step (4) repeatedly stops to drop into the potassium primary phosphate powder when the mass ratio of ultrapure water and potassium primary phosphate powder reaches 1:0.5-0.7 in reactor, keeps reactor temperature at 30-135 ℃, and stirs 1-2 hour.
2. the method for dissolving phosphoric acid potassium dihydrogen powder according to claim 1, it is characterized in that: described reactor is outside equipped with the spiral uprising shape heating tube, and reactor heats reactor by the thermal oil in the heating tube.
3. the method for dissolving phosphoric acid potassium dihydrogen powder according to claim 1 is characterized in that: in described step (3), when reactor temperature reaches 115 ℃, the potassium primary phosphate powder is dropped in the reactor.
4. the method for dissolving phosphoric acid potassium dihydrogen powder according to claim 1, it is characterized in that: in described step (5), the mass ratio of ultrapure water and potassium primary phosphate powder reaches 1:0.625.
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| CN2012103396923A CN102862965A (en) | 2012-09-14 | 2012-09-14 | Method of dissolving monopotassium phosphate powder |
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| CN2012103396923A CN102862965A (en) | 2012-09-14 | 2012-09-14 | Method of dissolving monopotassium phosphate powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106315533A (en) * | 2016-08-05 | 2017-01-11 | 常熟市圆启晶体材料有限公司 | Recrystallization and dissolution method for crude monopotassium phosphate |
| CN110372418A (en) * | 2019-06-04 | 2019-10-25 | 四川络布新材料科技有限公司 | A kind of instant powder potassium dihydrogen phosphate and its preparation facilities and centrifugal spray dryer drying process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1519397A (en) * | 2003-09-01 | 2004-08-11 | 山东大学 | Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category |
-
2012
- 2012-09-14 CN CN2012103396923A patent/CN102862965A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1519397A (en) * | 2003-09-01 | 2004-08-11 | 山东大学 | Method and equipment for growing large sectional monocrystal of potassium dihydrogen phosphate category |
Non-Patent Citations (1)
| Title |
|---|
| 白炳贤等: "滴定法测定磷酸二氢钾的溶解度", 《河南师范大学学报》, no. 1, 31 December 1988 (1988-12-31), pages 124 - 127 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106315533A (en) * | 2016-08-05 | 2017-01-11 | 常熟市圆启晶体材料有限公司 | Recrystallization and dissolution method for crude monopotassium phosphate |
| CN110372418A (en) * | 2019-06-04 | 2019-10-25 | 四川络布新材料科技有限公司 | A kind of instant powder potassium dihydrogen phosphate and its preparation facilities and centrifugal spray dryer drying process |
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Application publication date: 20130109 |