CN108190917A - A kind of preparation process for industrializing top pure grade ammonium bromide - Google Patents
A kind of preparation process for industrializing top pure grade ammonium bromide Download PDFInfo
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- CN108190917A CN108190917A CN201711389488.1A CN201711389488A CN108190917A CN 108190917 A CN108190917 A CN 108190917A CN 201711389488 A CN201711389488 A CN 201711389488A CN 108190917 A CN108190917 A CN 108190917A
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- Prior art keywords
- ammonium bromide
- ammonium
- pure grade
- top pure
- bromination
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/166—Ammonium bromide
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of preparation processes for industrializing top pure grade ammonium bromide, belong to Inorganic synthese field.It is characterized in that：Step is as follows：(1) bromination aqueous ammonium is prepared, deionized water is squeezed into ammonium bromide reaction kettle, it opens ammonium bromide solution circulating pump and beats cycle, the logical ammonia valve door of control makes temperature be no more than 50 DEG C, bromine is added in when pH value reaches 9.5, solution pH value in ammonium bromide reaction kettle is made to be maintained at 8.0 8.5, temperature is no more than 60 DEG C, obtains bromination aqueous ammonium；(2) ammonium bromide solution is purified, outlet valve is opened, bromination aqueous ammonium is made first to be purified through granular activated carbon filter core, then to condensing crystallizing in flash concentration tank；(3) top pure grade ammonium bromide is made, condensing crystallizing liquid is put into centrifuge and carries out separation of solid and liquid, obtains ammonium bromide crystal, then through drying, obtain top pure grade bromination ammonium product.The preparation process of top pure grade ammonium bromide of the present invention is more advanced, has that product yield is big, purity is high, and production cost is low, suitable for industrialized production.
Description
Technical field
The invention belongs to Inorganic synthese field, especially a kind of preparation process for industrializing top pure grade ammonium bromide.
Background technology
Ammonium bromide is a kind of relatively broad fine chemicals of purposes, it is photosensitive industrially be used as photographic film, printing paper and
Photosensitive emulsifier is used for the chemical analysis reagent of titrimetry copper in analytical chemistry, is used as wood fire retardant in timber industry,
It is used as sedative in medicine, is the oral medicine of neurasthenia and epilepsy etc..There are many method for preparing ammonium bromide, can use examination grade agent
Bromine hydracid and the ammonium bromide of ammonium hydrogen carbonate synthetic agent grade and photograph can also use industrial bromine, industrial urea, technical grade carbon
The ammonium bromide of sour hydrogen ammonium " one-step method " production SILVER REAGENT and photograph, but these methods are all difficult to produce the ammonium bromide of top pure grade,
And need the ammonium bromide using top pure grade in pharmaceutical industry.
Patent 201310279842 discloses a kind of preparation method of top pure grade ammonium bromide, and this method includes putting distilled water
Enter in plastic barrel, be passed through ammonia and ammonium hydroxide is made；By bromine in ammonium hydroxide obtained is slowly added with stirring, then proceed to be passed through ammonia
Gas is reaction end, obtains clear solution to PH=7-8；Clear solution heating is concentrated into certain density and then passes through centrifugation
Machine filters while hot, obtains ammonium bromide crystal；Obtained ammonium bromide is dried, obtains top pure grade finished product.According to comparing, this is specially
Profit has larger difference with above patent document.
Invention content
It is an object of the invention to overcome the shortage of prior art, according to the described technical problem of above-mentioned background technology, carry
For the preparation work of industrialization top pure grade ammonium bromide that a kind of processing step is simple, production efficiency is high, impurity content is low, purity is high
Skill.
The present invention realizes that purpose technical solution is：
A kind of preparation process for industrializing top pure grade ammonium bromide, includes the following steps：
(1) bromination aqueous ammonium is prepared
Quantitative deionized water is squeezed into ammonium bromide reaction kettle, is then turned on ammonium bromide solution circulating pump and proceeds by follow
Ring, cycle are then turned on cooling water and logical ammonia valve door after 2-5 minutes, and ammonium bromide reaction kettle is controlled by leading to the open degree of ammonia valve door
It is no more than 50 DEG C in the temperature display numerical value of temperature measurer, when ammonium bromide reaction kettle starts to add when PH is counted and shown that pH value reaches 9.5
Enter bromine, control the aperture size of logical bromine valve so that solution pH value is maintained at 8.0-8.5 in ammonium bromide reaction kettle, and temperature is not
More than 60 DEG C, bromination aqueous ammonium is just obtained；
(2) ammonium bromide solution is purified
After bromination aqueous ammonium content reaches requirement concentration, outlet valve is opened, and control certain aperture, make ammonium bromide water
Solution first passes through granular activated carbon filter core and is purified, and removes bromate that may be present, hypobromite etc., then enters back into sudden strain of a muscle
It steams in concentration tank and carries out condensing crystallizing；
(3) top pure grade ammonium bromide is made
When there is mass crystallization in flash concentration tank, stop concentration, concentrate is put into centrifuge and carries out solid-liquid point
From obtaining ammonium bromide crystal, then ammonium bromide crystal is dried, obtain top pure grade bromination ammonium product.
Preferably, pressure is preferably controlled between -0.07MPa to -0.09MPa in flash concentration tank in the step (2).
It advantages of the present invention and has the beneficial effect that：
1st, a kind of preparation process of top pure grade ammonium bromide of the present invention is more advanced, and ammonium bromide reaction kettle, flash concentration tank are
Industrial processing equipment, and each equipment produces and uses and does not all have security risk, suitable for industrialized production, step is simple, production
Site work environment safety, easy to operate, comprehensive production cost is relatively low；
2nd, flash concentration tank, centrifuge, seed activity used in a kind of preparation process of top pure grade ammonium bromide of the present invention
Filtration core can ensure the refining effect of product, and device therefor condenser, flash concentration tank, centrifuge be by Electronic control,
With the features such as product yield is big, product purity is high, and technique is easy to automation, serialization.
Description of the drawings
Fig. 1 is a kind of equipment connection diagram for the preparation process for industrializing top pure grade ammonium bromide of the present invention.
Specific embodiment
The preferred embodiment of the present invention is illustrated below in conjunction with Fig. 1, it should be understood that preferred implementation described herein
Example is merely to illustrate and explain the present invention, and is not intended to limit the present invention.
A kind of embodiment 1, preparation process for industrializing top pure grade ammonium bromide, includes the following steps：
(1) bromination aqueous ammonium is prepared
Quantitative deionized water is squeezed into ammonium bromide reaction kettle, is then turned on ammonium bromide solution circulating pump and proceeds by follow
Ring, cycle are then turned on cooling water and logical ammonia valve door after 2-5 minutes, and ammonium bromide reaction kettle is controlled by leading to the open degree of ammonia valve door
It is no more than 50 DEG C in the temperature display numerical value of temperature measurer, when ammonium bromide reaction kettle starts to add when PH is counted and shown that pH value reaches 9.5
Enter bromine, control the aperture size of logical bromine valve so that solution pH value is maintained at 8.0-8.5 in ammonium bromide reaction kettle, and temperature is not
More than 60 DEG C, bromination aqueous ammonium is just obtained；
(2) ammonium bromide solution is purified
After bromination aqueous ammonium content reaches requirement concentration, outlet valve is opened, and control certain aperture, make ammonium bromide water
Solution first passes through granular activated carbon filter core and is purified, and removes bromate that may be present, hypobromite etc., then enters back into sudden strain of a muscle
It steams in concentration tank and carries out condensing crystallizing；
(3) top pure grade ammonium bromide is made
When there is mass crystallization in flash concentration tank, stop concentration, concentrate is put into centrifuge and carries out solid-liquid point
From obtaining ammonium bromide crystal, then ammonium bromide crystal is dried, obtain top pure grade bromination ammonium product.
Preferably, pressure is preferably controlled between -0.07MPa to -0.09MPa in flash concentration tank in the step (2).
A kind of embodiment 2, preparation process for industrializing top pure grade ammonium bromide, includes the following steps：
(1) bromination aqueous ammonium is prepared
300L deionized waters are squeezed into the ammonium bromide reaction kettle of 500L, be then turned on ammonium bromide solution circulating pump and start to follow
Ring, cycle are then turned on cooling water and logical ammonia valve door after 2 minutes, ammonium bromide reaction kettle are controlled to exist by leading to the open degree of ammonia valve door
The temperature display numerical value of temperature measurer is 45 DEG C, and bromine is initially added into when the online PH meters of ammonium bromide reaction kettle show that pH value reaches 9.5
Element controls the aperture size of logical bromine valve so that and solution pH value is maintained at 8.5 in ammonium bromide reaction kettle, and temperature is controlled at 55 DEG C,
Obtain bromination aqueous ammonium；
(2) ammonium bromide solution is purified
After bromination aqueous ammonium content reaches requirement concentration, outlet valve is opened, and control certain aperture, make ammonium bromide water
Solution first passes through granular activated carbon filter core and is purified, and removes bromate that may be present, hypobromite etc., then enters back into sudden strain of a muscle
It steams and condensing crystallizing is carried out in concentration tank, pressure control is in -0.08MPa in flash concentration tank；
(3) top pure grade ammonium bromide is made
When there is mass crystallization in flash concentration tank, stop concentration, concentrate is put into centrifuge and carries out solid-liquid point
From obtaining ammonium bromide crystal, then ammonium bromide crystal is dried, obtain top pure grade bromination ammonium product.
A kind of embodiment 3, preparation process for industrializing top pure grade ammonium bromide, includes the following steps：
(1) bromination aqueous ammonium is prepared
200L deionized waters are squeezed into the ammonium bromide reaction kettle of 300L, be then turned on ammonium bromide solution circulating pump and start to beat
Cycle, cycle are then turned on cooling water and logical ammonia valve door after 4 minutes, and ammonium bromide reaction kettle is controlled by leading to the open degree of ammonia valve door
It is 50 DEG C in the temperature display numerical value of temperature measurer, is initially added into when the online PH meters of ammonium bromide reaction kettle show that pH value reaches 9.0
Then bromine controls the aperture size of logical bromine valve so that solution pH value is maintained at 8.0 in ammonium bromide reaction kettle, temperature control
At 60 DEG C, bromination aqueous ammonium is obtained；
(2) ammonium bromide solution is purified
After bromination aqueous ammonium content reaches requirement concentration, outlet valve is opened, and control certain aperture, make ammonium bromide water
Solution first passes through granular activated carbon filter core and is purified, and removes bromate that may be present, hypobromite etc., then enters back into sudden strain of a muscle
It steams and condensing crystallizing is carried out in concentration tank, pressure control is in -0.09MPa in flash concentration tank；
(3) top pure grade ammonium bromide is made
When there is mass crystallization in flash concentration tank, stop concentration, concentrate is put into centrifuge and carries out solid-liquid point
From obtaining ammonium bromide crystal, then ammonium bromide crystal is dried, obtain top pure grade bromination ammonium product.
Finally it should be noted that：The foregoing is merely the preferred embodiments of the present invention, are not intended to restrict the invention, to the greatest extent
Pipe is with reference to the foregoing embodiments described in detail the present invention, for those skilled in the art, still can be with
It modifies to the technical solution recorded in foregoing embodiments or equivalent replacement is carried out to which part technical characteristic.It is all
Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in the guarantor of the present invention
Within the scope of shield.
Claims (2)
1. a kind of preparation process for industrializing top pure grade ammonium bromide, which is characterized in that step is as follows：
(1) bromination aqueous ammonium is prepared
Quantitative deionized water is squeezed into ammonium bromide reaction kettle, ammonium bromide solution circulating pump is then turned on and proceeds by cycle, follow
Ring is then turned on cooling water and logical ammonia valve door after 2-5 minutes, ammonium bromide reaction kettle is controlled to survey by leading to the open degree of ammonia valve door
The temperature display numerical value of Wen Yi is no more than 50 DEG C, when ammonium bromide reaction kettle is initially added into bromine when PH is counted and shown that pH value reaches 9.5
Element controls the aperture size of logical bromine valve so that solution pH value is maintained at 8.0-8.5 in ammonium bromide reaction kettle, and temperature is no more than
60 DEG C, just obtain bromination aqueous ammonium；
(2) ammonium bromide solution is purified
After bromination aqueous ammonium content reaches requirement concentration, outlet valve is opened, and control certain aperture, make bromination aqueous ammonium
It first passes through granular activated carbon filter core to be purified, removes bromate that may be present, hypobromite etc., it is dense then to enter back into flash distillation
Condensing crystallizing is carried out in contracting tank；
(3) top pure grade ammonium bromide is made
When there is mass crystallization in flash concentration tank, stop concentration, concentrate is put into centrifuge and carries out separation of solid and liquid, is obtained
It is dried to ammonium bromide crystal, then by ammonium bromide crystal, obtains top pure grade bromination ammonium product.
2. a kind of preparation process for industrializing top pure grade ammonium bromide according to claim 1, it is characterised in that：Step (2)
Pressure is preferably controlled between -0.07MPa to -0.09MPa in middle flash concentration tank.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711389488.1A CN108190917A (en) | 2017-12-21 | 2017-12-21 | A kind of preparation process for industrializing top pure grade ammonium bromide |
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| CN201711389488.1A CN108190917A (en) | 2017-12-21 | 2017-12-21 | A kind of preparation process for industrializing top pure grade ammonium bromide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942655A (en) * | 2019-04-29 | 2019-06-28 | 宜昌东阳光药业股份有限公司 | A kind of continuous crystallisation process of erythromycin thiocyanate crude product |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5290531A (en) * | 1992-03-18 | 1994-03-01 | Tetra Technologies, Inc. | Method of making ammonium bromide and calcium bromide |
| CN103395802A (en) * | 2013-07-05 | 2013-11-20 | 天津市化学试剂研究所 | Preparation method of ammonium bromide guaranteed reagent |
-
2017
- 2017-12-21 CN CN201711389488.1A patent/CN108190917A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5290531A (en) * | 1992-03-18 | 1994-03-01 | Tetra Technologies, Inc. | Method of making ammonium bromide and calcium bromide |
| CN103395802A (en) * | 2013-07-05 | 2013-11-20 | 天津市化学试剂研究所 | Preparation method of ammonium bromide guaranteed reagent |
Non-Patent Citations (3)
| Title |
|---|
| 克里斯蒂安•戈特沙克: "《水和废水臭氧氧化 臭氧及其应用指南》", 31 May 2004 * |
| 姜信真: "《化工生产基础知识》", 30 September 1983 * |
| 萧莹，龙明武: "《致富化工产品生产技术》", 31 August 1995 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109942655A (en) * | 2019-04-29 | 2019-06-28 | 宜昌东阳光药业股份有限公司 | A kind of continuous crystallisation process of erythromycin thiocyanate crude product |
| CN109942655B (en) * | 2019-04-29 | 2020-05-12 | 宜昌东阳光药业股份有限公司 | Continuous crystallization method of erythromycin thiocyanate crude product |
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Application publication date: 20180622 |