CN104192863A - Pilot plant test method in ammonium hydrogen fluoride production technology - Google Patents
Pilot plant test method in ammonium hydrogen fluoride production technology Download PDFInfo
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- CN104192863A CN104192863A CN201410420539.2A CN201410420539A CN104192863A CN 104192863 A CN104192863 A CN 104192863A CN 201410420539 A CN201410420539 A CN 201410420539A CN 104192863 A CN104192863 A CN 104192863A
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- ammonium bifluoride
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Abstract
The invention discloses a pilot plant test method in an ammonium hydrogen fluoride production technology. The pilot plant test method in the ammonium hydrogen fluoride production technology comprises the following steps of adding ammonium hydrogen fluoride mother liquor into a reaction kettle, respectively metering liquid hydrogen fluoride and liquid ammonia and putting the metered liquid hydrogen fluoride and liquid ammonia into the reaction kettle, and carrying out neutralization chemical reaction; turning on a cooling water return water inlet valve, starting an air compressor, and supplying the air into a bubbling pipe in a crystallizer; pumping hot ammonium hydrogen fluoride material cooled to 75-85 DEG C into a cooling crystallization kettle, introducing circulating cooling water into a cooling coil in the cooling crystallization kettle, carrying out forced cooling, and separating out ammonium hydrogen fluoride crystals; turning on an outlet valve of the cooling crystallization kettle, sending cooled material into a horizontal type spiral centrifugal machine to be subjected to spin-drying at constant speed, and packaging into finished products after inspection is passed. The pilot plant test method in the ammonium hydrogen fluoride production technology has the advantages that processing steps are simple and convenient, crystallization time is shortened by changing an ammonium hydrogen fluoride crystallization manner, and detection efficiency and production efficiency are improved.
Description
technical field
The middle method for testing that the present invention relates to a kind of ammonium bifluoride production technique, belongs to chemical production field.
Background technology
Ammonium bifluoride is a kind of corrosive chemical substance that has, wet, water decomposition poisonous fluorochemical, oxynitride and ammonia gas.Water-soluble is weak acid, can dissolve glass, is slightly soluble in alcohol, is very easily dissolved in cold water, and very easy deliquescence.Ammonium bifluoride can be used as chemical reagent, glass etching agent (participate in hydrofluoric acid with), fermentation industry sterilizing agent and sanitas, by the solvent of beryllium oxide metallic beryllium processed and the surface treatment agent of silicon steel sheet, also for the manufacture of pottery, magnesium alloy, the cleaning detergency of boiler feed water system and steam generation systems, and the acid treatment of oil field sandstone, also as alkylation, isomerization catalyst component.
Summary of the invention
The object of the invention is to provide a kind of middle method for testing for ammonium bifluoride production process, in time the product of producing is detected, so that expanding production.
The solution of the present invention is as follows: a kind of middle method for testing of ammonium bifluoride production technique, comprises the following steps:
A, in reactor, to add massfraction be 30-60% ammonium bifluoride mother liquor, and the liquid hydrogen fluoride that is 2-4:1 by mol ratio and liquefied ammonia measure respectively to be put in reactor, in generation and chemical reaction; In reaction process, temperature is controlled at 100-200 ℃; When reaction finishes, temperature is controlled at 90-100 ℃, and is cooled to 75-85 ℃;
B, open water coolant and enter backwater valve, start air compressor machine, start to bubbling pipe air feed in crystallizer;
C, with pump, be cooled to the ammonium bifluoride thermal material of 75-85 ℃ to squeeze in crystallisation by cooling still temperature, with the spiral coil cooling tube that the recirculated cooling waters of 15 ℃-30 ℃ pass in crystallisation by cooling still, force cooling, utilize the pressurized air that air compressor machine is sent into force to stir simultaneously, after 12～18 hours, fully be cooled to 30-50 ℃, ammonium bifluoride crystallization;
D, open cooling crystallization kettle outlet valve, at the uniform velocity cooled material is delivered in horizontal spiral centrifuge and dried, after the assay was approved, get final product packaging final prod.
Further, the ammonium bifluoride thermal material that completes reaction in described step a is cooled to 80 ℃.
Further, in described step c, in crystallisation by cooling still, the cooling rate of material is controlled at 0-4 ℃/h.
Further, bubbling blast main and spiral coil cooling tube are installed in described crystallisation by cooling still bottom, utilize air bubbling, allow the ammonium bifluoride particle of crystallization not be stained with shallow lake in bottom, are convenient to the continuous operation of next process centrifuge dripping.
Further, described crystallisation by cooling still bottom is provided with mother liquor receiving tank, the collection of material while changing valve or bottom valve leakage for tackling.
Beneficial effect of the present invention:
1, the present invention is in order to shorten crystallization time, the change to ammonium bifluoride crystallization mode, and, there is not chemical reaction in the change of crystallization mode, does not change the character of material.In implementation process, in crystallization kettle bottom, mother liquor receiving tank is installed, when valve or bottom valve leakage are changed in reply, the collection of material, possesses safe reliability.
2, novel process has been done change to the type selecting of whizzer.What old technology was selected is 3-foot loading and unloading material whizzer, and the direct material of operator, in handling material when turnover, must tightly have been dressed safety appliance, and manipulation strength is large, to operative employee's physical fitness requirement and heat-resisting require high.The horizontal spiral centrifuge that is that novel process adopts, the practicable continuous charging and discharging of this model whizzer, device housings is totally-enclosed, and operator directly do not contact material, semi-automatic operation, safe reliability is higher.
3, bubbling blast main and spiral coil cooling tube are installed in crystallisation by cooling still bottom, utilize air bubbling, allow the ammonium bifluoride particle of crystallization not be stained with shallow lake in bottom, are convenient to the continuous operation of next process centrifuge dripping.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
The equipment using in embodiment is as shown in table 1.
The device inventory using in table 1, embodiment.
Embodiment 1
A, in reactor, to add massfraction be 30% ammonium bifluoride mother liquor, and the liquid hydrogen fluoride that is 2:1 by mol ratio and liquefied ammonia measure respectively to be put in reactor, in generation and chemical reaction; In reaction process, temperature is controlled at 120 ℃; When reaction finishes, temperature is controlled at 80 ℃, and is cooled to 75 ℃;
B, open water coolant and enter backwater valve, start air compressor machine, start to bubbling pipe air feed in crystallizer;
C, with pump, be cooled to the ammonium bifluoride thermal material of 75-85 ℃ to squeeze in crystallisation by cooling still temperature, with the spiral coil cooling tube that the recirculated cooling waters of 30 ℃ pass in crystallisation by cooling still, force cooling, utilize the pressurized air that air compressor machine is sent into force to stir simultaneously, after 18 hours, fully be cooled to 50 ℃, ammonium bifluoride crystallization; In crystallisation by cooling still, the cooling rate of material is controlled at 0-4 ℃/h;
D, open cooling crystallization kettle outlet valve, at the uniform velocity cooled material is delivered in horizontal spiral centrifuge and dried, after the assay was approved, get final product packaging final prod.
Example example 2
A, in reactor, to add massfraction be 60% ammonium bifluoride mother liquor, and the liquid hydrogen fluoride that is 4:1 by mol ratio and liquefied ammonia measure respectively to be put in reactor, in generation and chemical reaction; In reaction process, temperature is controlled at 200 ℃; When reaction finishes, temperature is controlled at 100 ℃, and is cooled to 85 ℃;
B, open water coolant and enter backwater valve, start air compressor machine, start to bubbling pipe air feed in crystallizer;
C, with pump, be cooled to the ammonium bifluoride thermal material of 75-85 ℃ to squeeze in crystallisation by cooling still temperature, with the spiral coil cooling tube that the recirculated cooling waters of 15 ℃ pass in crystallisation by cooling still, force cooling, utilize the pressurized air that air compressor machine is sent into force to stir simultaneously, after 12 hours, fully be cooled to 30 ℃, ammonium bifluoride crystallization; In crystallisation by cooling still, the cooling rate of material is controlled at 0-4 ℃/h;
D, open cooling crystallization kettle outlet valve, at the uniform velocity cooled material is delivered in horizontal spiral centrifuge and dried, after the assay was approved, get final product packaging final prod.
Embodiment 3
A, in reactor, to add massfraction be 50 ammonium bifluoride mother liquors, and the liquid hydrogen fluoride that is 3:1 by mol ratio and liquefied ammonia measure respectively to be put in reactor, in generation and chemical reaction; In reaction process, temperature is controlled at 160 ℃; When reaction finishes, temperature is controlled at 95 ℃, and is cooled to 80 ℃;
B, open water coolant and enter backwater valve, start air compressor machine, start to bubbling pipe air feed in crystallizer;
C, with pump, be cooled to the ammonium bifluoride thermal material of 80 ℃ to squeeze in crystallisation by cooling still temperature, with the spiral coil cooling tube that the recirculated cooling waters of 20 ℃ pass in crystallisation by cooling still, force cooling, utilize the pressurized air that air compressor machine is sent into force to stir simultaneously, after 16 hours, fully be cooled to 40 ℃, ammonium bifluoride crystallization; In crystallisation by cooling still, the cooling rate of material is controlled at 0-4 ℃/h;
D, open cooling crystallization kettle outlet valve, at the uniform velocity cooled material is delivered in horizontal spiral centrifuge and dried, after the assay was approved, get final product packaging final prod.
Each embodiment products obtained therefrom performance index see the following form 2.
The measurement result of table 2, embodiment products obtained therefrom index
| Sample | Ammonium bifluoride content (%) | The dry amount (%) of burning | Ignition residue content (%) |
| Premium grads | ≧97 | ≦3 | ≦0.2 |
| First grade | ≧95 | ≦5 | ≦0.2 |
| Embodiment 1 | 98.6 | 0.6 | 0.061 |
| Embodiment 2 | 99.5 | 0.5 | 0.044 |
| Embodiment 13 | 99 | 0．7 | 0.058 |
As seen from the table, the quality product in embodiment 1-3 has all reached the level of top grade product.And above-described embodiment test products is analyzed through laboratory, all meet the requirement of industrial hydrogen fluoride GB28655-2012 target level of product quality.
Although above the specific embodiment of the present invention has been given to describe in detail and explanation; but what should indicate is; we can carry out various equivalences to above-mentioned embodiment according to conception of the present invention and change and revise; when its function producing does not exceed spiritual that specification sheets contains yet, all should be within protection scope of the present invention.
Claims (5)
1. a middle method for testing for ammonium bifluoride production technique, is characterized in that, comprises the following steps:
A, in reactor, to add massfraction be 30-60% ammonium bifluoride mother liquor, and the liquid hydrogen fluoride that is 2-4:1 by mol ratio and liquefied ammonia measure respectively to be put in reactor, in generation and chemical reaction; In reaction process, temperature is controlled at 100-200 ℃; When reaction finishes, temperature is controlled at 90-100 ℃, and is cooled to 75-85 ℃;
B, open water coolant and enter backwater valve, start air compressor machine, start to bubbling pipe air feed in crystallizer;
C, with pump, be cooled to the ammonium bifluoride thermal material of 75-85 ℃ to squeeze in crystallisation by cooling still temperature, with the spiral coil cooling tube that the recirculated cooling waters of 15 ℃-30 ℃ pass in crystallisation by cooling still, force cooling, utilize the pressurized air that air compressor machine is sent into force to stir simultaneously, after 12～18 hours, fully be cooled to 30-50 ℃, ammonium bifluoride crystallization;
D, open cooling crystallization kettle outlet valve, at the uniform velocity cooled material is delivered in horizontal spiral centrifuge and dried, after the assay was approved, get final product packaging final prod.
2. the middle method for testing of a kind of ammonium bifluoride production technique according to claim 1, is characterized in that the ammonium bifluoride thermal material that completes reaction in described step a is cooled to 80 ℃.
3. the middle method for testing of a kind of ammonium bifluoride production technique according to claim 1, is characterized in that, in described step c, in crystallisation by cooling still, the cooling rate of material is controlled at 0-4 ℃/h.
4. the middle method for testing of a kind of ammonium bifluoride production technique according to claim 1, it is characterized in that described crystallisation by cooling still bottom installation bubbling blast main and spiral coil cooling tube, utilize air bubbling, allow the ammonium bifluoride particle of crystallization not be stained with shallow lake in bottom, be convenient to the continuous operation of next process centrifuge dripping.
5. the middle method for testing of a kind of ammonium bifluoride production technique according to claim 1, is characterized in that described crystallisation by cooling still bottom is provided with mother liquor receiving tank, the collection of material while changing valve or bottom valve leakage for tackling.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105014083A (en) * | 2015-06-08 | 2015-11-04 | 中铝广西有色金源稀土股份有限公司 | Hydrogen resource recycling device for rare earth permanent magnetic material and application method of hydrogen resource recycling device |
| CN106152813A (en) * | 2015-04-03 | 2016-11-23 | 东至天孚化工有限公司 | A kind of ammonium acid fluoride water cooling tower |
| CN106145160A (en) * | 2015-04-03 | 2016-11-23 | 东至天孚化工有限公司 | A kind of ammonium acid fluoride production method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066767A (en) * | 2007-05-25 | 2007-11-07 | 浙江三美化工股份有限公司 | Improved wet process and apparatus for producing ammonium bifluoride |
| CN103803584A (en) * | 2012-11-08 | 2014-05-21 | 福建省邵武市永飞化工有限公司 | Ammonium bifluoride preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066767A (en) * | 2007-05-25 | 2007-11-07 | 浙江三美化工股份有限公司 | Improved wet process and apparatus for producing ammonium bifluoride |
| CN103803584A (en) * | 2012-11-08 | 2014-05-21 | 福建省邵武市永飞化工有限公司 | Ammonium bifluoride preparation method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106152813A (en) * | 2015-04-03 | 2016-11-23 | 东至天孚化工有限公司 | A kind of ammonium acid fluoride water cooling tower |
| CN106145160A (en) * | 2015-04-03 | 2016-11-23 | 东至天孚化工有限公司 | A kind of ammonium acid fluoride production method |
| CN105014083A (en) * | 2015-06-08 | 2015-11-04 | 中铝广西有色金源稀土股份有限公司 | Hydrogen resource recycling device for rare earth permanent magnetic material and application method of hydrogen resource recycling device |
| CN105014083B (en) * | 2015-06-08 | 2017-03-08 | 中铝广西有色金源稀土股份有限公司 | A kind of rare earth permanent-magnetic material hydrogen resource circulation utilizing device and its application process |
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Application publication date: 20141210 |