CN1326771C - Production method of ammonium iodide - Google Patents
Production method of ammonium iodide Download PDFInfo
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- CN1326771C CN1326771C CNB2005100219077A CN200510021907A CN1326771C CN 1326771 C CN1326771 C CN 1326771C CN B2005100219077 A CNB2005100219077 A CN B2005100219077A CN 200510021907 A CN200510021907 A CN 200510021907A CN 1326771 C CN1326771 C CN 1326771C
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Abstract
The present invention provides a novel method for producing ammonium iodides, particularly a method for producing ammonium iodides by using iodine, iron powders and ammonium bicarbonate as raw materials, which comprises a ferrous iodide preparing step, an ammonium iodide preparing step, a sulfate removing step, a suction filtration concentrating step and a crystallizing step in sequence, wherein in the ammonium iodide preparing step, ferrous iodides react with ammonium bicarbonate solution to generate ferrous carbonate, ammonium iodides, carbon dioxide and water, and ammonium iodides are prepared through a post-treatment step. In the present invention, substances with poor volatility and low corrosiveness, such as iodine, iron powders and ammonium bicarbonate are used as raw materials for producing ammonium iodides, requirements for producing devices are low, and corrosion preventing maintenance doesn't need to be carried out frequently. The producing process is easy to control, the producing environments are improved obviously, and the raw materials are easy to obtain. As a result, the production cost is much lowered.
Description
Technical field
The present invention proposes a kind of new ammonium iodide production method, is the method for raw material production ammonium iodide with iodine, iron powder, bicarbonate of ammonia specifically.
Background technology
Ammonium iodide is easily deliquescence four directions crystallization of white, be exposed to easily flavescence in the air, relative density 2.514,220 ℃ of boiling points (in a vacuum), heating (551 ℃) is then decomposed and is distilled, and water-soluble, pure, acetic acid, ammonia, is slightly soluble in ether, photosensitivity is arranged, be used to make the raw material of inorganic iodide, make the sensitive emulsion of photographic film and negative, medicine industry is used to make expectorant and diuretic(s).Usually the production method of ammonium iodide has following two kinds:
1. direct method
With ammoniacal liquor and iodine is raw material, prepares ammonium iodide in the presence of hydrogen peroxide
The shortcoming of this method is: because use liq ammonia, hydrogen peroxide, all be big, the easy decomposition of volatility, unsettled material, cause temperature of reaction to require to be higher than normal temperature, thereby increase the volatilization of ammoniacal liquor, hydrogen peroxide, iodine, come therefrom, working condition is difficult to control as: ingredient proportion, feed intake order and the number of times that feeds intake, pitch time, temperature of reaction; Production environment is poor, according to the requirement of chemical industry workshop safe limit, NH
3≤ 30mg/m
3, I
2≤ 1mg/m
3, H
2O
2≤ 1mg/m
3, this requirement is difficult to reach in production environment, can cause bigger harm to producers when serious, and security is relatively poor; As changing, must carry out confined reaction, absorb volatilization gas, will cause the increase of production cost again from this.
2. neutralisation
With liquid ammonia and hydroiodic acid HI is the feedstock production ammonium iodide
Its shortcoming is: this liquid ammonia, and character decision operating environments such as the instability of hydroiodic acid HI (HI), volatile, corrodibility are poor; The instability of hydroiodic acid HI and corrodibility have also determined to produce preparation hydroiodic acid HI complex process, need special corrosion-resistant specific equipment to produce, and often need carry out rotproofing, thereby cause the cost height.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art and provide that a kind of technology is simple, reaction is easy to control, equipment requirements is not high, raw material is easy to get, the production method of good work environment, ammonium iodide that cost is low.
The object of the present invention is achieved like this:
A kind of production method of ammonium iodide, it comprises preparation process, the preparation process of ammonium iodide, suction filtration, condensing crystal, the baking step of iron iodide successively, wherein,
A, iron iodide preparation process: with iodine and iron powder iodine in molar ratio: iron powder=1.0: 1.2-1.5 batching, join respectively in the container of water, wherein in the container weight amount of water be iodine weight 2-3 doubly, at temperature 40-60 ℃, stirring velocity is reaction 30-50 minute under 60-100 rev/min the condition, make iron iodide solution, measure free-iodine and IO
3 -Qualified, reaction finishes.Free-iodine and IO
3 -Measuring method press 2005 editions NaI standard tests of the Pharmacopoeia of the People's Republic of China, promptly get iron iodide solution 2ml, after adding the cold water 10ml that newly boiled and rising, add 2 of dilute sulphuric acids and starch indicating liquid 0.2ml, lucifuge is placed, and solution does not show blue in 2 minutes, and it is qualified to be;
B, ammonium iodide preparation process: the iron iodide for preparing is added in the ammonium bicarbonate soln, wherein, the mol ratio of iron iodide and bicarbonate of ammonia is 1.0: 2.0-2.3, under 60-100 rev/min stirring and 80-100 ℃ of temperature condition, reacted 30-50 minute, reaction generates iron protocarbonate precipitation, ammonium iodide, carbonic acid gas and water, measures free-iodine and IO
3 -After qualified, adjusting the solution pH value with bicarbonate of ammonia is that 6.5-7 gets final product, and measures free-iodine and IO
3 -Method and a in identical;
C, suction filtration, condensing crystal, drying step: the gac that adds the 2-5% that throws iodine amount (weight) in reaction solution stirred 20 minutes, suction filtration is removed iron protocarbonate precipitation and other impurity, the ammonium iodide evaporative crystallization of removing impurity, oven dry promptly gets the ammonium iodide product.
Wherein, iron iodide preparation process, suction filtration, condensing crystal, drying step all are common processes, with " the content unanimity that inorganic chemicals industry handbook (press publishes second edition in June, 1996 by chemical industry industry) is announced.
Wherein, reaction formula is as follows:
Because the material that the present invention adopts is iodine, iron powder, these volatility of bicarbonate of ammonia are little, corrodibility is low is the raw material production ammonium iodide, require low to production unit, need not carry out regular anticorrosion maintenance, production process control is very easy, production environment be improved significantly, and these raw materials are easy to get, thereby greatly reduce production cost.
Embodiment
Below by specific embodiment the present invention is described in further detail, but the present invention has more than and is limited to these examples.Below the bicarbonate of ammonia of Cai Yonging is the food grade bicarbonate of ammonia (GB1888-1998) that Zigong City letter crane chemical plant produces.
Embodiment 1: a kind of production method of pharmaceutical grade ammonium iodide, it comprise successively preparation process, the ammonium iodide of iron iodide preparation process, sulfate radical remove step, suction filtration enrichment step and crystallisation step, wherein,
A, iron iodide preparation process: with iodine and iron powder iodine in molar ratio: iron powder=1.0: 1.2 batchings, join respectively in the container of water, wherein the weight amount of water is 2 times of iodine weight in the container, 40 ℃ of temperature, stirring velocity is reaction 50 minutes under 60 rev/mins the condition, make iron iodide solution, measure free-iodine and IO
3 -Qualified, reaction finishes;
B, ammonium iodide preparation process: the iron iodide for preparing is added in the ammonium bicarbonate soln, wherein, the mol ratio of iron iodide and bicarbonate of ammonia is 1.0: 2.0, under 60 rev/mins stirrings and 80 ℃ of temperature condition, reacted 50 minutes, reaction generates iron protocarbonate precipitation, ammonium iodide, carbonic acid gas and water, measures free-iodine and IO
3 -After qualified, adjusting the solution pH value with bicarbonate of ammonia is 7 get final product mensuration free-iodine and IO
3 -Method and a in identical;
C, suction filtration, condensing crystal, drying step: 2% of adding throwing iodine amount (weight) gac stirred 20 minutes in reaction solution, and suction filtration is removed iron protocarbonate precipitation and other impurity, and the ammonium iodide evaporative crystallization of removing impurity, oven dry promptly gets the ammonium iodide product.
Embodiment 2: a kind of production method of pharmaceutical grade ammonium iodide, it comprise successively preparation process, the ammonium iodide of iron iodide preparation process, sulfate radical remove step, suction filtration enrichment step and crystallisation step, wherein,
A, iron iodide preparation process: with iodine and iron powder iodine in molar ratio: iron powder=1.0: 1.5 batchings, join respectively in the container of water, wherein the weight amount of water is 3 times of iodine weight in the container, 60 ℃ of temperature, stirring velocity is reaction 30 minutes under 100 rev/mins the condition, make iron iodide solution, measure free-iodine and IO
3 -Qualified, reaction finishes;
D, ammonium iodide preparation process: the iron iodide for preparing is added in the ammonium bicarbonate soln, wherein, the mol ratio of iron iodide and bicarbonate of ammonia is 1.0: 2.3, under 100 rev/mins stirrings and 100 ℃ of temperature condition, reacted 30 minutes, reaction generates iron protocarbonate precipitation, ammonium iodide, carbonic acid gas and water, measures free-iodine and IO
3 -After qualified, adjusting the solution pH value with bicarbonate of ammonia is 6.5 get final product mensuration free-iodine and IO
3 -Method and a in identical;
B, suction filtration, concentrated, drying step: 5% of adding throwing iodine amount (weight) gac stirred 20 minutes in reaction solution, and suction filtration is removed iron protocarbonate precipitation and other impurity, the ammonium iodide evaporative crystallization of removing impurity, dried and promptly got the ammonium iodide product.
The ammonium iodide product that adopts the present invention to make is checked (according to former HGB3197-60) by analysis, the results are shown in following table, meets or exceeds a grade chemical pure index, meets the chemical reagent standard.
| Project | HGB3197-60 | Embodiment 1 | Embodiment 2 |
| NH 4I/％， ≥ | 96.0％ | 99.0 | 99.2 |
| Water-insoluble %≤ | 0.01 | 0.01 | 0.007 |
| Ignition residue %≤ | 0.02 | 0.01 | 0.009 |
| Chlorion %≤ | 0.02 | 0.015 | 0.02 |
| Iodate and iodine %≤ | 0.01 | 0.005 | 0.008 |
| Alkalescence test %≤ | 0.003 | 0.003 | 0.001 |
Claims (1)
1, a kind of production method of ammonium iodide, it comprises preparation process, the preparation process of ammonium iodide, suction filtration, condensing crystal, the baking step of iron iodide successively, the preparation process that it is characterized in that ammonium iodide is that the iron iodide that will prepare adds in the ammonium bicarbonate soln, wherein the mol ratio of iron iodide and bicarbonate of ammonia is 1.0: 2.0-2.3,60-100 rev/min of stirring velocity and 80-100 ℃ of following the reaction 30-50 minute, reaction generates iron protocarbonate, ammonium iodide, carbonic acid gas and water, measures free-iodine and I0
3 -After qualified, adjusting the pH value of solution value with bicarbonate of ammonia is that 6.5-7 gets final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100219077A CN1326771C (en) | 2005-10-18 | 2005-10-18 | Production method of ammonium iodide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100219077A CN1326771C (en) | 2005-10-18 | 2005-10-18 | Production method of ammonium iodide |
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| Publication Number | Publication Date |
|---|---|
| CN1751998A CN1751998A (en) | 2006-03-29 |
| CN1326771C true CN1326771C (en) | 2007-07-18 |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134083B (en) * | 2011-05-06 | 2012-08-22 | 天津市科密欧化学试剂有限公司 | Production method of ammonium iodide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4921688A (en) * | 1987-09-18 | 1990-05-01 | Hoechst Aktiengesellschaft | Process for preparing ammine salts of aluminum iodide |
| CN1346331A (en) * | 1999-03-29 | 2002-04-24 | 霍尼威尔专用化学品希尔兹有限公司 | Method for producing high-purity solutions using gaseous hydrogen fluoride |
| CN1554586A (en) * | 2003-12-22 | 2004-12-15 | 云南三环化工有限公司 | Process for preparing ammonium hydrogen fluoride |
-
2005
- 2005-10-18 CN CNB2005100219077A patent/CN1326771C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4921688A (en) * | 1987-09-18 | 1990-05-01 | Hoechst Aktiengesellschaft | Process for preparing ammine salts of aluminum iodide |
| CN1346331A (en) * | 1999-03-29 | 2002-04-24 | 霍尼威尔专用化学品希尔兹有限公司 | Method for producing high-purity solutions using gaseous hydrogen fluoride |
| CN1554586A (en) * | 2003-12-22 | 2004-12-15 | 云南三环化工有限公司 | Process for preparing ammonium hydrogen fluoride |
Non-Patent Citations (1)
| Title |
|---|
| 硫酸亚铁制硫酸钾的研究 卢芳仪等，硫酸工业，第3期 1999 * |
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