CN109250689A - It is a kind of rinsed using secondary zinc oxide after the salt water technique for preparing calcium iodate as raw material - Google Patents
It is a kind of rinsed using secondary zinc oxide after the salt water technique for preparing calcium iodate as raw material Download PDFInfo
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- CN109250689A CN109250689A CN201811441999.8A CN201811441999A CN109250689A CN 109250689 A CN109250689 A CN 109250689A CN 201811441999 A CN201811441999 A CN 201811441999A CN 109250689 A CN109250689 A CN 109250689A
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- iodine
- zinc oxide
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- calcium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/22—Oxygen compounds of iodine
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention relates to it is a kind of rinsed using secondary zinc oxide after the salt water technique for preparing calcium iodate as raw material, comprising the following steps: (1) secondary zinc oxide rinsing salt water is evaporated concentration, centrifugation obtains water containing salt compounded of iodine;(2) hydrochloric acid is added to water containing salt compounded of iodine, hydrogen peroxide is then added dropwise, the pH value of system is in 1-2, when no iodine generates, terminates reaction, filtering obtains iodine mud;(3) lye is added into iodine mud, reaction solution pH is 8 ~ 9, and stirring and dissolving, filtering obtains Biodine;(4) solution of chlorate is prepared, Biodine is then added dropwise thereto, it is 85-90 degrees Celsius that the pH value of system, which is less than or equal to 1, temperature, and when reaction solution is colourless, reaction terminates, and filtering obtains acid iodide hydrogen salt solution;(5) be added calcium salt reaction production calcium iodate, filtering, after Washing of Filter Cake, drying to get.Technical process of the invention realizes the closed production of iodine, and technique, equipment are simple, and economic cost is low, is suitble to industrialization automated production.
Description
Technical field
The present invention relates to calcium iodate preparation process more particularly to it is a kind of rinsed using secondary zinc oxide after salt water as raw material prepare
The technique of calcium iodate.
Background technique
Iodine is the base stock of the inorganic and organic iodide of manufacture, and is human body and the essential nutrient of plant,
Also have been widely used in terms of national defence and sophisticated technology.Iodine is important one of biological element, it is the composition of thyroxine
There is an adjustment effect in part to the metabolic rate of organism, and iodine deficiency can cause Thyroid Gland Swell, under basal metabolic rate and vigor
Drop, therefore be widely used in feed additive production.At present the additive of iodine mainly have potassium iodide, sodium iodide, Potassiumiodate and
Calcium iodate etc., but preceding several iodide less stables are precipitated iodine and reduce life as potassium iodide and sodium iodide are easily oxidized
Object potency, but calcium iodate, since solubility is low, property is stablized, and also supplements calcium salt while supplementing iodine, is by current state
The inside and outside feed addictive being widely recognized as.The current technique for preparing calcium iodate is usually by iodine using after oxidizing
Salt is reacted into calcium salt, since iodine is readily volatilized, not only operation difficulty is big, is also easy to that iodine loss and iodine volatilization is caused to draw
The environmental pollution risen.
Therefore, a new calcium iodate preparation approach has been started, has been had great importance.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies, provide it is a kind of rinsed with secondary zinc oxide after salt water for original
The technique that material prepares calcium iodate.
To achieve the goals above, the technical solution adopted by the present invention is as follows:
A method of the salt water after being rinsed using secondary zinc oxide prepares calcium iodate as raw material, specifically includes the following steps:
Step 1 is concentrated by evaporation: secondary zinc oxide rinsing salt water being evaporated concentration, until Baume degrees is 50, is then centrifuged for, is separated
Recycle chlorate, gained centrifuge mother liquor, i.e. water containing salt compounded of iodine;The existence form of iodine is iodized salt in the water containing salt compounded of iodine, described to contain
The content of iodized salt is 0.5-1% in salt compounded of iodine water;
Step 2, iodine analysis: being added hydrochloric acid to water containing salt compounded of iodine obtained by step 1, and adjusting pH value is 1-2, is then slowly added dropwise thereto double
Oxygen water is stirred when being added dropwise, while the pH value of maintenance system monitors the generation of iodine in reaction solution in 1-2, reaction process
Situation when no iodine generates, terminates reaction;Then it filters, obtains liquor B and filter cake B, gained filter cake B is solid iodine mud;The iodine
The content of iodine is 70-80% in mud;
Step 3, purification: obtaining that lye is added immediately in iodine mud to step 2, and adjusting and controlling reaction solution pH is 8 ~ 9, stirring
Then 30min filters to dissolving, obtains liquor C, i.e. Biodine;In the Biodine existence form of iodine be iodized salt and
Iodate, iodized salt and iodate total concentration are 10-16% in the Biodine;
Step 4, oxidation: it firstly, preparing solution of chlorate, adjusts pH value to after being less than or equal to 1, is heated to 85-90 degrees Celsius, then
Slowly Biodine made from a dropping step 4 thereto while stirring, in reaction process, the pH value for controlling reaction system is less than etc.
It is 85-90 degrees Celsius in 1, temperature, when reaction solution is colourless in adition process, stops being added dropwise, reaction terminates, and filters, obtains filtrate
D, the filtrate D are acid iodide hydrogen salt solution;The content of acid iodide hydrogen salt is 10% in the acid iodide hydrogen salt solution;It is described insoluble
Impurity includes sulphur simple substance;
Step 5, synthesis: the molar ratio by iodate ion and calcium ion is 2:1, is added into step 4 gained acid iodide hydrogen salt solution
Enter calcium salt reaction production calcium iodate, control reaction system PH is 6-7, is stirred to react 30min, filters, obtains filtrate E and filter cake E, institute
It states after filter cake E is washed with water, dries to get one water calcium iodate of feed grade;A water calcium iodate in the one water calcium iodate of feed grade
Content be greater than 99.3%.
Further, the yield of the water calcium iodate is greater than 90%.
Further, the volumetric concentration of hydrochloric acid used is 30% in step 2;The mass concentration of hydrogen peroxide used is 28%;
The additional amount for the hydrogen peroxide that mass concentration is 28% in step 2 are as follows: the dioxygen that water containing salt compounded of iodine is 28% with the mass concentration
The volume ratio of water is 100:0.8 ~ 1.2;
The method that no iodine generates is judged in step 2: extracting reaction solution after filtering into test tube, hydrogen peroxide is added dropwise thereto, passes through mesh
The mode of survey is observed solution and is generated without iodine;
The mass concentration of lye is 10-15% in step 3;The lye uses sodium hydroxide solution or potassium hydroxide solution.
Further, also need to carry out step 0 rinsing before carrying out step 1 and being concentrated by evaporation: by secondary zinc oxide and water quality
Volume ratio 1g:2 ~ 5ml is measured, water is added into secondary zinc oxide, after stirring 1.5 ~ 2.5h, filters pressing obtains filtrate A, i.e., used in step 1
Secondary zinc oxide rinses salt water;
Further, step 2 iodine is analysed further include: after obtaining liquor B, is 8-9 by the liquor B tune PH, is then combined with to step
In rapid 0 gained filtrate A.
Further, step 5 synthesis further includes being 8-9 by the filtrate E tune PH, being then combined with after obtaining filtrate E
Into step 0 gained filtrate A.
Further, iodine analysis needs to operate continuously with filtering in step 2, and carries out in confined space, intermediate without pause, completes
Iodine analysis is filtered immediately.
Further, the mass concentration of solution of chlorate described in step 4 be 10%, the chlorate be sodium chlorate or
Potassium chlorate.
Further, the calcium salt is selected from one or more of calcium chloride, calcium hydroxide, calcium carbonate or calcium nitrate.
Further, the rate of addition that hydrogen peroxide is slowly added dropwise in the analysis of step 2 iodine are as follows: the water containing salt compounded of iodine of 1000mL corresponding 1 ~
The addition speed of 2mL/min, the water containing salt compounded of iodine of 2000mL then correspond to the addition speed of 2 × (1 ~ 2mL/min), and 1000L's contains iodine
Salt water then corresponds to the addition speed of 1 ~ 2L/min, and so on;
The rate of addition that Biodine is slowly added dropwise in step 4 oxidation are as follows: the corresponding 1 ~ 2.5mL/min's of the water containing salt compounded of iodine of 1000mL
Speed is added;The water containing salt compounded of iodine of 2000mL then corresponds to the addition speed of 2 × (1 ~ 2.5mL/min), and the water containing salt compounded of iodine of 1000L is then right
The addition speed of 1 ~ 2.5L/min is answered, and so on.
Chemical principle of the invention is as follows:
1. iodine is analysed: being the I that will contain in salt compounded of iodine water?Use hydrogen peroxide oxidation for elemental iodine in acid condition.
Chemical equation: 2I?+H2O2+2HCl=I2+2Cl--+2H2O;
2. purification: the iodine mud containing elemental iodine being dissolved using lye, is filtered, insoluble solid silt is removed, chemistry is anti-
Answer formula: 3I2+6OH?=5I?+IO3 ?-+3H2O;
3. oxidation: 5I?+IO3 ?+6HCl=6Cl?+3I2+3H2O;
I2+2ClO3 ?+HCl =H(IO3)2 ?+Cl?+Cl2↑;
During this, moment is oxidized to iodate after iodine occurs;
4. synthesis: H (IO3)2 ?+CaCl2+OH?= 2Cl?+Ca(IO3)2.H2O
Compared with prior art, advantages of the present invention are as follows:
(1) of the invention is concentrated feed liquid before producing iodine, not only completes the recycling of chlorate, also to produce iodine for the first time
The operation that elemental iodine is isolated by filtration afterwards is possibly realized, required equipment it is simple, compared with air absorption process, ion-exchange etc.
It more easily realizes and industrializes closed production, avoid or reduce the distillation of iodine in iodine mud, and because of environmental problem caused by iodine distillation;
(2) it after producing iodine, is dissolved immediately using lye, and progress pipeline transportation, its solution are more steady in the form of sodium iodate and sodium iodide
Fixed, transport is more convenient, operation is simpler, and iodine utilization rate height, almost free of losses, (3) potassium chlorate or sodium chlorate are as oxidant
Oxidation reaction is carried out, is reacted in the form of sodium iodate and sodium iodide with chlorate, entire oxidation process does not occur iodine (oxidation
Moment is oxidized to iodate solution after iodine occurs in the process, stablizes, easy to operate, quick), relatively using iodine with
For chloric acid reactant salt, the utilization rate of iodine is higher, avoids the distillation of iodine, and because iodine distillation caused by environmental problem;This hair
Bright being used cooperatively by this three step process, so that the preparation process of entire calcium iodate may be implemented closed production, simple process,
Economic cost is lower, production safety, environmental protection, convenient.
It is existing production calcium iodate technology compare, the present invention rinsed using secondary zinc oxide after salt water as raw material, with hydrogen peroxide
For oxidant, hydrochloric acid tune pH value carries out the oxidization enrichment of iodine, and mentioning the mother liquor after iodine is sodium chloride or potassium chloride, is not generated new
Waste maintains the benign cycle of whole system;Iodine mud after producing iodine is purified, oxidation, synthesis obtain the feed grade greater than 99%
Calcium iodate not only solves using secondary zinc oxide as raw material and produces discharge of wastewater in sulfuric acid zinc technology, causes the problem of environmental pollution,
A kind of new raw material for preparing calcium iodate has also been started, waste is enable to turn waste into wealth, has compensated for and is floated using production zinc sulfate
Wash water prepares the blank of calcium iodate, provides a new approach for the synthesis calcium iodate of health environment-friendly.
Contain a small amount of silt and other impurities in secondary zinc oxide rinsing salt water of the present invention, passes through primary centrifugation or mistake
Filter be difficult to remove it is clean, the Process fusion that the present invention removes the removal of silt and impurity entire calcium iodate preparation process in
It (during (1) recycles chlorate, is centrifuged through being concentrated by evaporation, partial impurities can be removed, (2) purification step can remove portion
Divide impurity, (3) hypochlorite oxidation removes partial impurities in the process), it avoids independent secondary zinc oxide rinsing salt water impurity removal process and leads
The problem of process flow of cause increases, increased costs.
Iodine analysis and filtering and second of iodine analysis and filtering of the present invention are both needed to be carried out continuously, and can reduce disappearing for hydrogen peroxide
Consumption improves the oxygenation efficiency of hydrogen peroxide, and the oxygenation efficiency for avoiding the oxidation of hydrogen peroxide caused by the peroxidating of iodine from obtaining iodine is low
The problem of.
The present invention need each reagent of strict control addition sequence, be added speed, additional amount, reaction temperature, reaction pH and
The rate of addition of the judgement of reaction end, the especially rate of addition of hydrogen peroxide and the reaction end of oxidation reaction and Biodine,
With dropwise addition sequence, reagent consumption minimum can be reached by carrying out operation using parameter disclosed by the invention, and yield is maximum, realizes drop
The purpose of low process costs.
Technical process of the invention realizes the closed production of iodine, and simple process, economic cost is lower, production safety, ring
Solution after guarantor, convenient synthesis calcium iodate is chlorate, and can enter salt extraction system, not increase new impurity, maintain whole
The benign cycle of a system, equipment is simple, easy to operate, is very suitable to industrialization automated production.
Detailed description of the invention
Fig. 1 is the process flow chart of one embodiment of the invention.
Specific embodiment
Further details of narration is carried out to the present invention with reference to embodiments.
Embodiment 1
It is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material, specifically includes the following steps:
Step 1, rinsing: pressing secondary zinc oxide and water quality volume ratio 1g:3.5ml, and water is added into secondary zinc oxide, after stirring 2h,
Filters pressing obtains filtrate A, the salt water after the filtrate A, i.e. secondary zinc oxide rinsing;
Step 2 is concentrated by evaporation: the salt water after the rinsing of step 1 gained secondary zinc oxide being carried out multiple-effect evaporation concentration, until Baume degrees is
50, it is then centrifuged for, separation and recovery chlorination potassium and sodium chloride, gained centrifuge mother liquor, i.e. water containing salt compounded of iodine, iodine in the water containing salt compounded of iodine
Existence form is sodium iodide and potassium iodide, I in the water containing salt compounded of iodine?Content be 0.8%;
Step 3, iodine analysis: the hydrochloric acid that volumetric concentration is 30% is added to water containing salt compounded of iodine obtained by step 2, adjusting pH value is 1-2, then
The volume ratio for the hydrogen peroxide for being 28% by water containing salt compounded of iodine and mass concentration is 100:0.8 ~ 1.2;Mass concentration is slowly added dropwise thereto
It for 28% hydrogen peroxide, is stirred when being added dropwise, while the pH value of maintenance system monitors iodine in reaction solution in 1-2, reaction process
Generation situation, extract reaction solution filtering after into test tube, hydrogen peroxide is added dropwise thereto, solution is observed by way of range estimation without iodine
It generates, at this point, reaction is terminated, it can (reaction time about 30min);It filters immediately after, obtains liquor B and filter cake B, the filtrate
B tune PH is incorporated into step 1 gained filtrate A after being 8-9, and gained filter cake B is solid iodine mud;Iodine contains in the iodine mud
Amount is 75%;The rate of addition of hydrogen peroxide being slowly added dropwise are as follows: the water containing salt compounded of iodine of 1000mL corresponds to the addition speed of 1.5mL/min;
The water containing salt compounded of iodine of 2000mL then corresponds to the addition speed of 2 × 1.5mL/min, and the water containing salt compounded of iodine of 2000L then corresponds to 2 × 1.5L/min
Addition speed, and so on;
Step 4, purification: the lye (alkali described in the present embodiment that mass concentration is 12% is added immediately into the iodine mud that step 3 obtains
Liquid is sodium hydroxide solution), adjusting and controlling reaction solution pH is 8 ~ 9, and stirring 30min is to dissolving, and then filtering removes silt and alkali
Insoluble impurities (secondary zinc oxide rinses in salt water through other resulting solid impurities of hydrogen peroxide oxidation), obtains liquor C, i.e., molten containing iodine
Liquid, the existence form of iodine is iodized salt and iodate in the Biodine, and iodized salt and iodate are total in the Biodine
Concentration is 13%;
Step 6, oxidation: firstly, preparing the solution of chlorate that mass concentration is 10%, (chlorate described in the present embodiment is chloric acid
Potassium), it adjusts pH value to after being less than or equal to 1, is heated to 85-90 degrees Celsius, then slowly a dropping step 5 is made thereto while stirring
Biodine, in reaction process, it is 85-90 degrees Celsius that the pH value for controlling reaction system, which is less than or equal to 1, temperature, works as dropwise addition
When reaction solution is colourless in the process, stop being added dropwise, reaction terminates, is filtered to remove insoluble impurities (predominantly sulphur simple substance), obtains filtrate
D, the filtrate D are acid iodide hydrogen salt solution, and the content of acid iodide hydrogen salt is 10% in the acid iodide hydrogen salt solution;Biodine is slow
Slowly the rate of addition being added dropwise are as follows: the water containing salt compounded of iodine of 1000mL corresponds to the addition speed of 1.8mL/min;The water containing salt compounded of iodine of 2000mL is then
The addition speed of corresponding 2 × 1.8mL/min, and so on;
Step 7, synthesis: the molar ratio by iodate ion and calcium ion is 2:1, is added into step 6 gained acid iodide hydrogen salt solution
Enter calcium salt (calcium salt described in the present embodiment is calcium chloride) reaction production calcium iodate, control reaction system PH is 6-7, is stirred to react
30min, filtering are obtained after filtrate E and filter cake E, the filtrate E tune PH are 8-9 and are incorporated into step 1 gained filtrate A;The filter
After water washing 4 times of 2 volumes of cake E;The content of a water calcium iodate is greater than 99.7% in the feed grade calcium iodate.Using the work
Skill calcium iodate yield is 93%.
Embodiment described above is merely a preferred embodiment of the present invention, and the simultaneously exhaustion of the feasible implementation of non-present invention.It is right
For persons skilled in the art, any aobvious to made by it under the premise of without departing substantially from the principle of the invention and spirit and
The change being clear to should be all contemplated as falling within claims of the invention.
Claims (9)
1. it is a kind of rinsed using secondary zinc oxide after the salt water technique for preparing calcium iodate as raw material, which is characterized in that specifically include with
Lower step:
Step 1 is concentrated by evaporation: secondary zinc oxide rinsing salt water being evaporated concentration, until Baume degrees is 50, is then centrifuged for, is separated
Recycle chlorate, gained centrifuge mother liquor, i.e. water containing salt compounded of iodine;
Step 2, iodine analysis: being added hydrochloric acid to water containing salt compounded of iodine obtained by step 1, and adjusting pH value is 1-2, is then slowly added dropwise thereto double
Oxygen water is stirred when being added dropwise, while the pH value of maintenance system monitors the generation of iodine in reaction solution in 1-2, reaction process
Situation when no iodine generates, terminates reaction;Then it filters, obtains liquor B and filter cake B, gained filter cake B is solid iodine mud;
Step 3, purification: obtaining that lye is added immediately in iodine mud to step 2, and adjusting and controlling reaction solution pH is 8 ~ 9, stirring
Then 30min filters to dissolving, obtains liquor C, i.e. Biodine;
Step 4, oxidation: it firstly, preparing solution of chlorate, adjusts pH value to after being less than or equal to 1, is heated to 85-90 degrees Celsius, then
Slowly Biodine made from a dropping step 4 thereto while stirring, in reaction process, the pH value for controlling reaction system is less than etc.
It is 85-90 degrees Celsius in 1, temperature, when reaction solution is colourless in adition process, stops being added dropwise, reaction terminates, and filters, obtains filtrate
D, the filtrate D are acid iodide hydrogen salt solution;
Step 5, synthesis: the molar ratio by iodate ion and calcium ion is 2:1, is added into step 4 gained acid iodide hydrogen salt solution
Enter calcium salt reaction production calcium iodate, control reaction system PH is 6-7, is stirred to react 30min, filters, obtains filtrate E and filter cake E, institute
It states after filter cake E is washed with water, dries to get one water calcium iodate of feed grade.
2. it is according to claim 1 it is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material,
It is characterized in that, the volumetric concentration of hydrochloric acid used is 30% in step 2;The mass concentration of hydrogen peroxide used is 28%;
The additional amount for the hydrogen peroxide that mass concentration is 28% in step 2 are as follows: the dioxygen that water containing salt compounded of iodine is 28% with the mass concentration
The volume ratio of water is 100:0.8 ~ 1.2;
Judge the method that no iodine generates in step 2: extracting reaction solution after filtering into test tube, be added dropwise hydrogen peroxide thereto, solution without
Iodine generates;
The mass concentration of lye is 10-15% in step 3;The lye uses sodium hydroxide solution or potassium hydroxide solution.
3. it is according to claim 1 it is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material,
It is characterized in that, also needs to carry out step 0 rinsing before carrying out step 1 and being concentrated by evaporation: by secondary zinc oxide and water quality volume ratio
Water is added into secondary zinc oxide by 1g:2 ~ 5ml, and after stirring 1.5 ~ 2.5h, filters pressing obtains filtrate A, i.e. secondary zinc oxide used in step 1
Rinse salt water.
4. it is according to claim 3 it is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material,
It is characterized in that, the analysis of step 2 iodine further include: be 8-9 by the liquor B tune PH after obtaining liquor B, be then combined with to obtained by step 0
In filtrate A.
5. it is according to claim 3 it is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material,
It is characterized in that, it is 8-9 by the filtrate E tune PH that step 5 synthesis, which further includes after obtaining filtrate E, is then combined with to obtained by step 0
In filtrate A.
6. it is according to claim 1 it is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material,
It being characterized in that, iodine analysis needs to operate continuously with filtering in step 2, and carries out in confined space, and it is intermediate without pause, complete iodine analysis immediately
It is filtered.
7. it is according to claim 1 it is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material,
It is characterized in that, the mass concentration of solution of chlorate described in step 4 is 10%, and the chlorate is sodium chlorate or potassium chlorate.
8. it is according to claim 1 it is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material,
It is characterized in that, the calcium salt is selected from one or more of calcium chloride, calcium hydroxide, calcium carbonate or calcium nitrate.
9. it is according to claim 1 it is a kind of rinsed using secondary zinc oxide after salt water the technique of calcium iodate is prepared as raw material,
It is characterized in that, the rate of addition that hydrogen peroxide is slowly added dropwise in the analysis of step 2 iodine are as follows: the corresponding 1 ~ 2mL/min of the water containing salt compounded of iodine of 1000mL
Addition speed;The rate of addition that Biodine is slowly added dropwise in step 4 oxidation are as follows: the water containing salt compounded of iodine of 1000mL corresponding 1 ~
The addition speed of 2.5mL/min.
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