Production device of cuprous iodide

Abstract

The utility model belongs to the technical field of chemical reaction devices, and particularly relates to a production device of cuprous iodide. The production device of the cuprous iodide comprises a raw material tank, a first stirring tank, a reaction tank, a filtering and washing tower and drying equipment which are connected in sequence, the raw material tank comprises an aromatization stock solution storage tank, a sodium carbonate solution storage tank and a sodium sulfite storage tank; the aromatization stock solution storage tank, the sodium carbonate solution storage tank and the sodium sulfite storage tank are respectively communicated with the first stirring tank; and the reaction tank is also communicated with a copper sulfate solution storage tank. The utility model provides a production device of cuprous iodide, which aims at solving the problems of resource waste and difficulty in subsequent garbage treatment due to the fact that elemental iodine contained in an aromatization stock solution is treated as garbage in the prior art, takes the aromatization stock solution as a raw material, fully utilizes the elemental iodine in the aromatization stock solution and generates more expensive cuprous iodide.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical reaction devices, and more specifically relates to a production device for cuprous iodide. Background Art

[0002] Cuprous iodide (CuI) is a p-type semiconductor material with a wide bandgap (Eg = 3.1 eV). It is insoluble in water and has three crystalline phases: α, β, and γ. At low temperatures (below 350°C), it exists as a cubic γ-CuI crystal, with the iodine atom acting as both an electron acceptor and a hole vacancy. Between 350°C and 392°C, it exists as a fibrous mineral structure, β-CuI, making it an ionic conductor. Above 392°C, it exists as a cubic α-CuI structure, making it a mixed conductor. Cuprous iodide is widely used as a catalyst in organic synthesis (such as in the synthesis of Grignard reagents and the Heck reaction), a resin modifier (to improve resin performance and enhance its heat and chemical resistance), an artificial rain agent (to catalyze the formation of ice nuclei), anode ray tube covers (to protect the tube and improve its performance), and as a source of iodine in iodized salt.

[0003] Currently, there are many methods for preparing cuprous iodide. Common methods include the co-thermal reaction of copper and iodine, the reaction of copper and hydroiodic acid, and the co-thermal reaction of copper and iodoform. In addition, there are physical methods such as laser pulse precipitation, magnetron sputtering, and vacuum evaporation. However, these methods are complicated to operate, have long reaction times, low product yields, and produce a large amount of three wastes, making them unsuitable for industrial production. Precipitation and sol-gel methods are relatively simple to operate. The precipitation method uses an iodine salt as a precipitant, adding it to a salt solution containing metallic copper ions to undergo a chemical reaction. The main drawback of this method is that the reaction is divided into two steps during the preparation process: first, the iodine salt and a copper salt react to obtain copper iodide, and then the copper iodide is unstable in solution to prepare cuprous iodide. In the second step, a large amount of free iodine is generated, making product separation difficult, resulting in a decrease in iodine utilization and increased costs. In addition, the recovery rate of free iodine is not very high, resulting in a waste of iodine resources. Therefore, further development of a preparation method for cuprous iodide is particularly necessary. Summary of the Invention

[0004] The purpose of the utility model is to provide a device for recovering iodine element in aromatization raw liquid to generate cuprous iodide.

[0005] A cuprous iodide production device comprises a raw material tank, a No. 1 stirring tank, a reaction tank, a filtering and washing tower, and a drying device connected in sequence; the raw material tank comprises an aromatization stock solution storage tank, a sodium carbonate solution storage tank, and a sodium sulfite storage tank; the aromatization stock solution storage tank, the sodium carbonate solution storage tank, and the sodium sulfite storage tank are respectively connected to the No. 1 stirring tank; and the reaction tank is also connected to a copper sulfate solution storage tank.

[0006] In the existing industrial production of 3,5-dimethylphenol, the catalytic cracking step typically produces an aromatization solution (e.g., Chinese Patent Application No. CN 113443968 B). This solution contains approximately 6% iodine. Existing processes treat this solution as waste, resulting in wasteful resources and difficult subsequent waste disposal. The present invention utilizes the aromatization solution as a raw material and fully utilizes the iodine present.

[0007] The aromatization raw liquid, sodium carbonate solution and sodium sulfite react in a stirring tank No. 1, and the generated sodium iodide enters the reaction tank and reacts with the copper sulfate solution to obtain a cuprous iodide mixture. The cuprous iodide mixture enters the filter washing tower and is filtered, and then washed with water, washed with ethanol once, and washed with ethanol twice to obtain pure cuprous iodide. The pure cuprous iodide is produced after drying.

[0008] The reaction equation during the formation process is as follows:

[0009] Na2SO3+I2+Na2CO3=2NaI+Na2SO4+H2O+CO2;

[0010] 4NaI+2CuSO4=2CuI↓+2Na2SO4+I2.

[0011] Through the above two-step reaction, the iodine element in the aromatization raw solution is fully recovered to produce more expensive cuprous iodide.

[0012] In a preferred embodiment, the aromatization stock solution in the aromatization stock solution storage tank contains 4%-8% of elemental iodine.

[0013] In a preferred embodiment, the drying equipment is a negative pressure drying tank.

[0014] In a preferred embodiment, the liquid outlet of the filtering and washing tower is connected to the first stirring tank.

[0015] When sodium iodide and copper sulfate react to produce cuprous iodide, a small amount of elemental iodine is also produced. After washing with water, one ethanol wash, and a second ethanol wash, the iodine is separated from the cuprous iodide and dissolved in ethanol. The iodine-containing wash solution is returned to mixing tank No. 1, where it reacts with sodium sulfite and sodium carbonate to produce sodium iodide, further improving the recovery rate of elemental iodine.

[0016] In a preferred embodiment, the cuprous iodide production device further includes a No. 2 stirring tank and a distillation tower connected in sequence; the inlet of the No. 2 stirring tank is connected to the outlet of the No. 1 stirring tank; and the No. 2 stirring tank is also connected to a sodium chloride storage tank.

[0017] In a preferred embodiment, the water phase outlet of the No. 2 stirring tank is connected to the inlet of the No. 1 stirring tank;

[0018] The deiodinated aromatization solution enters the No. 2 stirring tank, where it is evenly mixed with sodium chloride to accelerate stratification. The oil phase primarily contains 3,5-dimethylphenol, which is distilled into the rectification tower to produce 3,5-dimethylphenol. The aqueous phase also contains small amounts of iodine and sodium iodide. After stratification, the aqueous phase re-enters the No. 1 stirring tank for reaction.

[0019] The advantages of this utility model are:

[0020] In response to the problem that the existing process treats the iodine contained in the aromatization raw liquid as waste, thereby causing waste of resources and making subsequent waste disposal difficult, the utility model provides a cuprous iodide production device. The aromatization raw liquid is used as a raw material, the iodine therein is fully utilized to produce the more expensive cuprous iodide, and the economic benefits of about 3 million yuan can be generated for the company each year. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is the production device of the utility model;

[0022] In the figure, 1-aromatization stock solution storage tank, 2-sodium carbonate solution storage tank, 3-sodium sulfite storage tank, 4-No. 1 stirring tank, 5-No. 2 stirring tank, 6-distillation tower, 7-copper sulfate solution storage tank, 8-reaction tank, 9-filtration washing tower, 10-drying equipment;

[0023] Figure 2 This is the production process of the utility model. DETAILED DESCRIPTION

[0024] The following is a detailed example and Figure 1 and Figure 2 The production device of the utility model is described in detail.

[0025] Example 1

[0026] A cuprous iodide production device comprises a raw material tank, a No. 1 stirring tank 4, a reaction tank 8, a filtering and washing tower 9, and a drying device 10 connected in sequence; the raw material tank comprises an aromatization stock solution storage tank 1, a sodium carbonate solution storage tank 2, and a sodium sulfite storage tank 3; the aromatization stock solution storage tank 1, the sodium carbonate solution storage tank 2, and the sodium sulfite storage tank 3 are respectively connected to the No. 1 stirring tank 4; and the reaction tank 8 is also connected to the copper sulfate solution storage tank 7.

[0027] The aromatization stock solution in the aromatization stock solution storage tank contains 6%-7% of elemental iodine.

[0028] The drying equipment 10 is a negative pressure drying tank. The liquid outlet of the filter-wash tower 9 is connected to the first stirring tank 4. The first stirring tank 4 is also connected to the second stirring tank 5 and the distillation tower 6. The inlet of the second stirring tank 5 is connected to the outlet of the first stirring tank 4. The water phase outlet of the second stirring tank 5 is connected to the inlet of the first stirring tank 4. The second stirring tank 5 is also connected to the sodium chloride storage tank 11.

[0029] In the utility model, the aromatization stock solution, the sodium carbonate solution and the sodium sulfite react in the first stirring tank 4, and the generated sodium iodide enters the reaction tank 8 to react with the copper sulfate solution to obtain a cuprous iodide mixture. The cuprous iodide mixture enters the filter washing tower 9 for filtration, and is washed with water, washed with ethanol once, and washed with ethanol twice to obtain pure cuprous iodide. The pure cuprous iodide is dried and then output.

[0030] After sodium iodide and copper sulfate react to generate cuprous iodide, a small amount of elemental iodine is also obtained. After washing with water, washing with ethanol once, and washing with ethanol twice, the iodine is separated from the cuprous iodide and dissolved in ethanol. The cleaning liquid containing the elemental iodine returns to the first stirring tank 4 from the filtering and washing tower 9, reacts with sodium sulfite and sodium carbonate to generate sodium iodide, further improving the recovery rate of the elemental iodine.

[0031] The deiodinated aromatization liquid enters the second stirring tank 5, where it is evenly mixed with sodium chloride to accelerate stratification. The oil phase primarily contains 3,5-dimethylphenol, which is distilled to the distillation tower 6 to produce 3,5-dimethylphenol. The aqueous phase also contains small amounts of iodine and sodium iodide. After stratification, the aqueous phase from the second stirring tank 5 re-enters the first stirring tank 4 for reaction.

[0032] As a result, about 6 tons of pure cuprous iodide can be produced each year, generating nearly 3 million yuan in economic benefits for the company.

[0033] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, and all of these should be included in the scope of the claims of the present invention.

Claims

1. A production device for cuprous iodide, characterized in that, The invention comprises a raw material tank, a No. 1 stirring tank, a reaction tank, a filter washing tower and a drying device which are connected in sequence; the raw material tank comprises an aromatization stock solution storage tank, a sodium carbonate solution storage tank and a sodium sulfite storage tank; the aromatization stock solution storage tank, the sodium carbonate solution storage tank and the sodium sulfite storage tank are respectively connected to the No. 1 stirring tank; the reaction tank is also connected to a copper sulfate solution storage tank.

2. The production device according to claim 1, characterized in that The aromatization stock solution in the aromatization stock solution storage tank contains 4%-8% of elemental iodine.

3. The production device according to claim 1, characterized in that The drying equipment is a negative pressure drying tank.

4. The production device according to claim 1, characterized in that The liquid outlet of the filtering and washing tower is communicated with the first stirring tank.

5. The production device according to any one of claims 1 to 4, characterized in that: The production device of cuprous iodide further comprises a No. 2 stirring tank and a distillation tower which are connected in sequence; the inlet of the No. 2 stirring tank is connected to the outlet of the No. 1 stirring tank; the No. 2 stirring tank is also connected to a sodium chloride storage tank.

6. The production device according to claim 5, characterized in that The water phase outlet of the No. 2 mixing tank is connected to the inlet of the No. 1 mixing tank.

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