CN109250689B - Process for preparing calcium iodate by taking saline water obtained after rinsing secondary zinc oxide as raw material - Google Patents
Process for preparing calcium iodate by taking saline water obtained after rinsing secondary zinc oxide as raw material Download PDFInfo
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- CN109250689B CN109250689B CN201811441999.8A CN201811441999A CN109250689B CN 109250689 B CN109250689 B CN 109250689B CN 201811441999 A CN201811441999 A CN 201811441999A CN 109250689 B CN109250689 B CN 109250689B
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Abstract
The invention relates to a process for preparing calcium iodate by taking saline water obtained after rinsing zinc hypoxide as a raw material, which comprises the following steps: (1) evaporating and concentrating the zinc hypoxide rinsing brine, and centrifuging to obtain iodine-containing brine; (2) adding hydrochloric acid into the iodine-containing saline water, then dropwise adding hydrogen peroxide, stopping the reaction when the pH value of the system is 1-2 and no iodine is generated, and filtering to obtain iodine mud; (3) adding alkali liquor into the iodine mud, wherein the pH value of reaction liquid is 8-9, stirring for dissolving, and filtering to obtain an iodine-containing solution; (4) preparing a chlorate solution, then dropwise adding an iodine-containing solution into the chlorate solution, finishing the reaction when the pH value of the system is less than or equal to 1 and the temperature is 85-90 ℃ and the reaction liquid is colorless, and filtering to obtain a hydrogen iodate solution; (5) adding calcium salt to react to produce calcium iodate, filtering, washing filter cake, and drying to obtain the final product. The technological process of the invention realizes the airtight production of iodine, has simple process and equipment and low economic cost, and is suitable for industrial automatic production.
Description
Technical Field
The invention relates to a preparation process of calcium iodate, in particular to a process for preparing calcium iodate by taking saline water obtained after rinsing zinc hypoxide as a raw material.
Background
Iodine is a basic raw material for preparing inorganic and organic iodides, is an indispensable nutrient element for human bodies and plants, and has wide application in national defense and advanced technologies. Iodine is one of important vital elements, is a component of thyroxine, has a regulating effect on the metabolism rate of organisms, and can cause goiter and decline of basal metabolism rate and activity due to iodine deficiency, so that the iodine is widely used in the production of feed additives. At present, the iodine additives mainly comprise potassium iodide, sodium iodide, potassium iodate, calcium iodate and the like, but the former iodides are not stable, for example, the potassium iodide and the sodium iodide are easy to be oxidized to separate out simple substance iodine so as to reduce the biological potency, but the calcium iodate has low solubility and stable property, supplements calcium salt while supplementing iodine, and is widely accepted feed additives at home and abroad at present. The existing process for preparing calcium iodate usually comprises the steps of oxidizing elemental iodine by using an oxidizing agent and then reacting the oxidized elemental iodine with calcium salt to form salt, wherein the elemental iodine is easy to volatilize, so that the operation difficulty is high, and the iodine loss and the environmental pollution caused by iodine volatilization are easy to cause.
Therefore, a new preparation way of calcium iodate is created, and the method has important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a process for preparing calcium iodate by taking saline water obtained after rinsing zinc hypoxide as a raw material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing calcium iodate by taking saline water obtained after rinsing zinc hypoxide as a raw material specifically comprises the following steps:
step 1, evaporation and concentration: evaporating and concentrating secondary zinc oxide rinsing brine until the Baume degree is 50, centrifuging, separating and recovering chloride, and obtaining centrifugal mother liquor, namely iodine-containing brine; the iodine in the iodine-containing saline exists in the form of iodized salt, and the content of the iodized salt in the iodine-containing saline is 0.5-1%;
step 2, iodization: adding hydrochloric acid into the iodine-containing saline water obtained in the step (1), adjusting the pH value to be 1-2, then slowly dripping hydrogen peroxide into the iodine-containing saline water, stirring while dripping, simultaneously maintaining the pH value of the system to be 1-2, monitoring the generation condition of the elementary iodine in the reaction liquid in the reaction process, and stopping the reaction when no iodine is generated; then filtering to obtain filtrate B and a filter cake B, wherein the filter cake B is solid iodine mud; the content of elementary iodine in the iodine mud is 70-80%;
and step 3, purification: immediately adding alkali liquor into the iodine mud obtained in the step 2, adjusting and controlling the pH value of a reaction solution to be 8-9, stirring for 30min until the reaction solution is dissolved, and then filtering to obtain a filtrate C, namely an iodine-containing solution; the iodine in the iodine-containing solution exists in the forms of iodide and iodate, and the total concentration of the iodide and the iodate in the iodine-containing solution is 10-16%;
step 4, oxidation: firstly, preparing a chlorate solution, adjusting the pH value to be less than or equal to 1, heating to 85-90 ℃, then slowly dripping the iodine-containing solution prepared in the step 4 into the chlorate solution while stirring, wherein the pH value of a reaction system is controlled to be less than or equal to 1 and the temperature is 85-90 ℃ in the reaction process, when the reaction solution is colorless in the addition process, the dripping is stopped, the reaction is finished, and filtering is carried out to obtain a filtrate D, wherein the filtrate D is the hydrogen iodate solution; the content of the iodate in the iodate solution is 10 percent; the insoluble impurities include elemental sulfur;
step 5, synthesis: adding calcium salt into the solution of the iodate obtained in the step 4 according to the molar ratio of iodate ions to calcium ions of 2:1 to react to produce calcium iodate, controlling the pH of a reaction system to be 6-7, stirring to react for 30min, filtering to obtain filtrate E and a filter cake E, washing the filter cake E with water, and drying to obtain feed-grade calcium iodate monohydrate; the content of calcium iodate monohydrate in the feed-grade calcium iodate monohydrate is more than 99.3 percent.
Further, the yield of the calcium iodate monohydrate is more than 90%.
Further, the volume concentration of the hydrochloric acid used in the step 2 is 30 percent; the mass concentration of the hydrogen peroxide is 28 percent;
the hydrogen peroxide with the mass concentration of 28% in the step 2 is added in the following amount: the volume ratio of the iodine-containing saline water to the 28% hydrogen peroxide is 100: 0.8-1.2;
the method for judging no iodine generation in the step 2 comprises the following steps: filtering the reaction solution, adding into a test tube, dropwise adding hydrogen peroxide, and observing the solution by visual observation to ensure that no iodine is generated;
in the step 3, the mass concentration of the alkali liquor is 10-15%; the alkali liquor adopts sodium hydroxide solution or potassium hydroxide solution.
Further, before performing step 1 evaporative concentration, step 0 rinsing is also required: according to the mass volume ratio of the secondary zinc oxide to the water of 1 g: 2-5 ml, adding water into the secondary zinc oxide, stirring for 1.5-2.5 h, and performing filter pressing to obtain a filtrate A, namely the rinsing brine of the secondary zinc oxide used in the step 1;
further, the step 2 of iodophoresis further comprises: after obtaining the filtrate B, adjusting the pH of the filtrate B to 8-9, and then combining the filtrate B with the filtrate A obtained in the step 0.
Further, the synthesis of step 5 further comprises, after obtaining filtrate E, adjusting the pH of the filtrate E to 8-9, and then combining the filtrate E with the filtrate A obtained in step 0.
Further, the iodization and the filtration in the step 2 need to be continuously operated, and are carried out in a closed space without pause in the middle, and the filtration is immediately carried out after the iodization is finished.
Further, in the step 4, the mass concentration of the chlorate solution is 10%, and the chlorate is 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, in the step 2, the dropping speed of the hydrogen peroxide in the iodophoresis process is as follows: the method comprises the following steps that 1000mL of the iodized saline corresponds to the adding speed of 1-2 mL/min, 2000mL of the iodized saline corresponds to the adding speed of 2 x (1-2 mL/min), 1000L of the iodized saline corresponds to the adding speed of 1-2L/min, and the like;
in the step 4, the slowly dropping speed of the iodine-containing solution in the oxidation is as follows: 1000mL of iodine-containing saline corresponds to the adding speed of 1-2.5 mL/min; 2000mL of the iodized saline corresponds to an addition rate of 2 x (1-2.5 mL/min), 1000L of the iodized saline corresponds to an addition rate of 1-2.5L/min, and so on.
The chemical reaction principle of the invention is as follows:
① iodization is carried out by dissolving I in iodine-containing saline－Under the acidic condition, hydrogen peroxide is used for oxidation to form iodine simple substance.
The chemical reaction formula is as follows: 2I－+H2O2+2HCl＝I2+2Cl－-+2H2O；
② purifying by dissolving iodine mud containing iodine with alkali solution, filtering, and removing insoluble solid silt, wherein the chemical reaction formula is 3I2+6OH－＝5I－+IO3 －-+3H2O；
③ Oxidation: 5I－+IO3 －+6HCl＝6Cl－+3I2+3H2O；
I2+2ClO3 －+HCl＝H(IO3)2 －+Cl－+Cl2↑；
In the process, the iodine is oxidized into iodate instantly after the iodine appears;
④ Synthesis of H (IO)3)2 －+CaCl2+OH－＝2Cl－+Ca(IO3)2.H2O
Compared with the prior art, the invention has the advantages that:
the method has the advantages that (1) the feed liquid is concentrated before iodine production, so that the recovery of chloride is completed, the operation of filtering and separating iodine simple substances after the iodine production for the first time becomes possible, the required equipment is simple, the industrial closed production is easier to realize than an air absorption method, an ion exchange method and the like, and the sublimation of iodine in the iodine mud and the environmental problem caused by iodine sublimation are avoided or reduced; (2) after iodine is produced, alkali liquor is adopted for dissolving immediately, and pipeline transportation is carried out in the form of sodium iodate and sodium iodide, so that the solution is more stable, the transportation is more convenient, the operation is simpler, the iodine utilization rate is high, and almost no loss exists, (3) potassium chlorate or sodium chlorate is used as an oxidizing agent for carrying out oxidation reaction, and the sodium iodate and the sodium iodide react with chlorate in the form of sodium iodate and sodium iodide, so that iodine does not appear in the whole oxidation process (the simple substance iodine is oxidized into an iodate solution instantly after appearing in the oxidation process, the operation is convenient and rapid), and compared with the reaction of the simple substance iodine and the chlorate, the iodine utilization rate is higher, and the sublimation of the iodine and the environmental problem caused by iodine sublimation are avoided; the invention can realize closed production in the whole preparation process of calcium iodate by matching the three steps of processes, and has the advantages of simple process, lower economic cost, safe, environment-friendly and convenient production.
Compared with the prior art for producing calcium iodate, the method takes the saline water after rinsing the secondary zinc oxide as a raw material, hydrogen peroxide as an oxidant, hydrochloric acid adjusts the pH value to carry out oxidation enrichment of iodine, and the mother solution after iodine extraction is sodium chloride or potassium chloride, so that new waste is not generated, and the virtuous circle of the whole system is kept; the feed-grade calcium iodate with the concentration of more than 99 percent is obtained by purifying, oxidizing and synthesizing the iodine sludge after iodine production, thereby not only solving the problems of waste water discharge and environmental pollution caused in the process of producing zinc sulfate by using zinc hypoxide as a raw material, but also creating a new raw material for preparing the calcium iodate, changing waste into valuable, making up the blank of preparing the calcium iodate by using the rinsing water for producing the zinc sulfate, and providing a new way for healthy and environment-friendly synthesis of the calcium iodate.
The secondary zinc oxide rinsing brine of the invention contains a small amount of silt and other impurities, which are difficult to be removed completely through one-time centrifugation or filtration, the invention integrates the silt removal and impurity removal processes into the whole calcium iodate preparation process ((1) in the process of recovering chloride, partial impurities can be removed through evaporation concentration centrifugation, (2) partial impurities can be removed in the purification step, and (3) partial impurities are removed in the chlorate oxidation process), thereby avoiding the problems of increased process flow and increased cost caused by the single secondary zinc oxide rinsing brine impurity removal process.
The invention has the advantages that the iodization and filtration as well as the secondary iodization and filtration are continuously carried out, the consumption of hydrogen peroxide can be reduced, the oxidation rate of the hydrogen peroxide is improved, and the problem of low oxidation rate of elemental iodine obtained by oxidation of the hydrogen peroxide caused by iodine peroxidation is solved.
The invention needs to strictly control the adding sequence, adding speed, adding amount, reaction temperature, reaction pH and reaction end point of each reagent, particularly the judgment of the dropping speed of hydrogen peroxide and the reaction end point of oxidation reaction, and the dropping speed and dropping sequence of iodine-containing solution.
The process realizes the closed production of iodine, has simple process, lower economic cost, safe and environment-friendly production, ensures that the solution after synthesizing the calcium iodate is the chlorate, can enter a salt extraction system, does not add new impurities, keeps the virtuous circle of the whole system, has simple equipment and convenient operation, and is very suitable for industrial automatic production.
Drawings
FIG. 1 is a process flow diagram of one embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A process for preparing calcium iodate by taking saline water obtained after rinsing zinc hypoxide as a raw material specifically comprises the following steps:
step 1, rinsing: according to the mass volume ratio of the secondary zinc oxide to the water of 1 g: 3.5ml, adding water into the zinc hypoxide, stirring for 2 hours, and performing filter pressing to obtain a filtrate A, wherein the filtrate A is the saline water obtained after rinsing the zinc hypoxide;
step 2, evaporation and concentration: performing multi-effect evaporation and concentration on the saline water obtained in the step 1 after rinsing the zinc hypoxide until the baume degree is 50, then centrifuging, separating and recovering potassium chloride and sodium chloride, wherein the obtained centrifugal mother solution is iodized saline water, iodine exists in the iodized saline water in the form of sodium iodide and potassium iodide, and I in the iodized saline water－The content of (A) is 0.8%;
step 3, iodizing: adding hydrochloric acid with the volume concentration of 30% into the iodine-containing saline water obtained in the step 2, adjusting the pH value to 1-2, and then adjusting the volume ratio of the iodine-containing saline water to hydrogen peroxide with the mass concentration of 28% to be 100: 0.8-1.2; slowly dripping 28% hydrogen peroxide solution into the reaction kettle while stirring, simultaneously maintaining the pH value of the system at 1-2, monitoring the generation condition of the elementary iodine in the reaction solution in the reaction process, filtering the reaction solution, then putting the reaction solution into a test tube, dripping the hydrogen peroxide solution into the reaction kettle, observing that the solution has no iodine generation in a visual inspection mode, and stopping the reaction (the reaction time is about 30 min); then immediately filtering to obtain a filtrate B and a filter cake B, adjusting the pH of the filtrate B to 8-9, and then merging the filtrate B into the filtrate A obtained in the step 1 to obtain the filter cake B, namely the solid iodine mud; the content of elemental iodine in the iodine mud is 75%; the dropping speed of the hydrogen peroxide is as follows: 1000mL of iodine-containing saline corresponds to the adding speed of 1.5 mL/min; 2000mL of the iodized saline corresponds to the adding speed of 2 multiplied by 1.5mL/min, 2000L of the iodized saline corresponds to the adding speed of 2 multiplied by 1.5L/min, and the like;
and 4, purification: adding an alkali liquor with the mass concentration of 12% (in the embodiment, the alkali liquor is a sodium hydroxide solution) into the iodine mud obtained in the step 3, adjusting and controlling the pH value of a reaction solution to be 8-9, stirring for 30min until the reaction solution is dissolved, and then filtering out silt and alkali insoluble impurities (other solid impurities obtained by oxidizing hydrogen peroxide in zinc hypoxide rinsing brine) to obtain a filtrate C, namely an iodine-containing solution, wherein iodine in the iodine-containing solution exists in the forms of iodide and iodate, and the total concentration of the iodide and iodate in the iodine-containing solution is 13%;
step 6, oxidation: firstly, preparing a chlorate solution (potassium chlorate in the embodiment) with the mass concentration of 10%, adjusting the pH value to be less than or equal to 1, heating to 85-90 ℃, then slowly dropwise adding the iodine-containing solution prepared in the step 5 while stirring, wherein in the reaction process, the pH value of a reaction system is controlled to be less than or equal to 1, the temperature is 85-90 ℃, when the reaction liquid is colorless in the dropwise adding process, the dropwise adding is stopped, the reaction is finished, insoluble impurities (mainly sulfur simple substance) are removed by filtration to obtain a filtrate D, the filtrate D is a hydrogen iodate solution, and the content of the hydrogen iodate in the hydrogen iodate solution is 10%; the dripping speed of the iodine-containing solution is as follows: 1000mL of iodine-containing saline corresponds to the adding speed of 1.8 mL/min; 2000mL of iodine-containing saline corresponds to the addition speed of 2X 1.8mL/min, and the rest can be done;
step 7, synthesis: adding calcium salt (calcium salt is calcium chloride in the embodiment) into the solution of the iodate obtained in the step 6 according to the molar ratio of iodate ions to calcium ions of 2:1 to react to produce calcium iodate, controlling the pH of a reaction system to be 6-7, stirring to react for 30min, filtering to obtain filtrate E and a filter cake E, adjusting the pH of the filtrate E to be 8-9, and combining the filtrate E with the filtrate A obtained in the step 1; the filter cake E was washed 4 times with 2 volumes of water; the content of calcium iodate monohydrate in the feed-grade calcium iodate is more than 99.7 percent. The yield of calcium iodate by adopting the process is 93 percent.
The embodiments described above are only preferred embodiments of the invention and are not exhaustive of the possible implementations of the invention. Any obvious modifications to the above would be obvious to those of ordinary skill in the art, but would not bring the invention so modified beyond the spirit and scope of the present invention.
Claims (9)
1. A process for preparing calcium iodate by taking saline water obtained after rinsing zinc hypoxide as a raw material is characterized by comprising the following steps:
step 1, evaporation and concentration: evaporating and concentrating secondary zinc oxide rinsing brine until the Baume degree is 50, centrifuging, separating and recovering chloride, and obtaining centrifugal mother liquor, namely iodine-containing brine;
step 2, iodization: adding hydrochloric acid into the iodine-containing saline water obtained in the step (1), adjusting the pH value to be 1-2, then slowly dripping hydrogen peroxide into the iodine-containing saline water, stirring while dripping, simultaneously maintaining the pH value of the system to be 1-2, monitoring the generation condition of the elementary iodine in the reaction liquid in the reaction process, and stopping the reaction when no iodine is generated; then filtering to obtain filtrate B and a filter cake B, wherein the filter cake B is solid iodine mud;
and step 3, purification: immediately adding alkali liquor into the iodine mud obtained in the step 2, adjusting and controlling the pH value of a reaction solution to be 8-9, stirring for 30min until the reaction solution is dissolved, and then filtering to obtain a filtrate C, namely an iodine-containing solution;
step 4, oxidation: firstly, preparing a chlorate solution, adjusting the pH value to be less than or equal to 1, heating to 85-90 ℃, then slowly dripping the iodine-containing solution prepared in the step 4 into the chlorate solution while stirring, wherein the pH value of a reaction system is controlled to be less than or equal to 1 and the temperature is 85-90 ℃ in the reaction process, when the reaction solution is colorless in the addition process, the dripping is stopped, the reaction is finished, and filtering is carried out to obtain a filtrate D, wherein the filtrate D is the hydrogen iodate solution;
step 5, synthesis: and (2) according to the molar ratio of iodate ions to calcium ions being 2:1, adding calcium salt or calcium hydroxide into the solution of the iodate obtained in the step (4) to react to produce calcium iodate, controlling the pH of a reaction system to be 6-7, stirring to react for 30min, filtering to obtain filtrate E and a filter cake E, washing the filter cake E with water, and drying to obtain the feed-grade calcium iodate monohydrate.
2. The process for preparing calcium iodate by using saline water obtained after rinsing zinc hypoxide as a raw material as claimed in claim 1, wherein the volume concentration of the hydrochloric acid used in the step 2 is 30%; the mass concentration of the hydrogen peroxide is 28 percent;
the hydrogen peroxide with the mass concentration of 28% in the step 2 is added in the following amount: the volume ratio of the iodine-containing saline water to the 28% hydrogen peroxide is 100: 0.8-1.2;
the method for judging no iodine generation in the step 2 comprises the following steps: filtering the reaction solution, adding into a test tube, and dropwise adding hydrogen peroxide into the reaction solution, wherein the solution is free of iodine;
in the step 3, the mass concentration of the alkali liquor is 10-15%; the alkali liquor adopts sodium hydroxide solution or potassium hydroxide solution.
3. The process for preparing calcium iodate from brine obtained after secondary zinc oxide rinsing as claimed in claim 1, wherein step 0 rinsing is further required before step 1 evaporative concentration: according to the mass volume ratio of the secondary zinc oxide to the water of 1 g: 2-5 ml, adding water into the zinc hypoxide, stirring for 1.5-2.5 h, and performing filter pressing to obtain a filtrate A, namely the rinsing brine of the zinc hypoxide used in the step 1.
4. The process of claim 3, wherein the iodizing step 2 further comprises: after obtaining the filtrate B, adjusting the pH of the filtrate B to 8-9, and then combining the filtrate B with the filtrate A obtained in the step 0.
5. The process of claim 3, wherein the step 5 further comprises adjusting the pH of the filtrate E to 8-9 after obtaining the filtrate E, and then combining the filtrate E with the filtrate A obtained in the step 0.
6. The process for preparing calcium iodate from brine obtained after rinsing zinc hypoxide as claimed in claim 1, wherein the iodization and filtration in step 2 are continuously performed in a closed space without pause, and the filtration is performed immediately after completion of the iodization.
7. The process for preparing calcium iodate by using saline water obtained after secondary zinc oxide rinsing as a raw material as claimed in claim 1, wherein the mass concentration of the chlorate solution in the step 4 is 10%, and the chlorate is sodium chlorate or potassium chlorate.
8. The process for preparing calcium iodate from brine obtained after secondary zinc oxide rinsing according to claim 1, wherein the calcium salt is selected from one or more of calcium chloride, calcium carbonate or calcium nitrate.
9. The process for preparing calcium iodate by using saline water obtained after rinsing zinc hypoxide as a raw material as claimed in claim 1, wherein the dropping speed of hydrogen peroxide in the iodophoresis in the step 2 is as follows: the addition speed of 1000mL of iodine-containing saline is 1-2 mL/min; in the step 4, the slowly dropping speed of the iodine-containing solution in the oxidation is as follows: 1000mL of iodine-containing saline corresponds to an addition rate of 1-2.5 mL/min.
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