CN112374530A - Preparation method of high-quality zinc sulfate monohydrate - Google Patents
Preparation method of high-quality zinc sulfate monohydrate Download PDFInfo
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- CN112374530A CN112374530A CN202011539880.1A CN202011539880A CN112374530A CN 112374530 A CN112374530 A CN 112374530A CN 202011539880 A CN202011539880 A CN 202011539880A CN 112374530 A CN112374530 A CN 112374530A
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- C01G9/00—Compounds of zinc
- C01G9/06—Sulfates
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Abstract
The embodiment of the invention provides a preparation method of high-quality zinc sulfate monohydrate, which relates to the technical field of compound preparation, and comprises the steps of dispersing zinc oxide in water, adding concentrated sulfuric acid for reaction, and filtering after the reaction to obtain reaction liquid; and adsorbing the reaction solution by using cation exchange resin, filtering and crystallizing to obtain high-quality zinc sulfate monohydrate. The preparation method has the advantages of cheap and easily-obtained raw materials, simple and convenient operation and low requirement on equipment, and can quickly and efficiently prepare the zinc sulfate monohydrate. And the produced zinc sulfate monohydrate product has high purity which reaches over 99 percent, the quality meets the national standard, the content of alkali metal and alkaline earth metal is less than or equal to 0.5 percent, and the zinc sulfate monohydrate can be widely applied to the fields of food and medicine.
Description
Technical Field
The invention relates to the technical field of compound preparation, in particular to a preparation method of high-quality zinc sulfate monohydrate.
Background
The molecular formula of zinc sulfate is ZnSO4It is colorless and odorless crystalline powder, is easily soluble in water, is less absorbed in stomach, is mainly absorbed by duodenum and small intestine, and is mostly combined with serum protein after entering blood. The zinc in the zinc sulfate is one of the essential trace elements for human body, and the zinc participates in the synthesis and activation of various enzymes and the synthesis of proteinThe regulation of adult cell growth, division and differentiation, and the growth and development of human body. Zinc deficiency in human body can cause various diseases, such as anorexia, anemia, growth retardation, nutritional dwarfism, enteropathic acrodermatitis and the like. During pregnancy, pregnant women also need to pay attention to zinc supplementation. Zinc sulfate can cause nausea, vomiting, etc., and is generally used in medicine for emetic, etc.
The zinc sulfate monohydrate can be widely applied to foods, dairy products, bread, biscuits, bean flour, health products and the like, and is used as an emetic in medicine.
The zinc sulfate monohydrate in the market is detected to find that the secondary detection items are unqualified, and the detection items mainly have the overproof problems of alkali metal and alkaline earth metal and have poor free-running property. Has poor application effect in the aspects of milk powder and premix.
Disclosure of Invention
The invention aims to provide a preparation method of zinc sulfate monohydrate, which has the advantages of cheap and easily-obtained raw materials, simple and convenient operation, low requirement on equipment, capability of quickly and efficiently preparing the zinc sulfate monohydrate and capability of effectively reducing the content of alkali metal and alkaline earth metal in the zinc sulfate monohydrate.
The embodiment of the invention is realized by the following steps:
a preparation method of high-quality zinc sulfate monohydrate comprises the following steps:
mixing zinc oxide with water to obtain a suspension;
slowly adding concentrated sulfuric acid into the suspension for reaction under continuous stirring, and filtering after the reaction is finished to obtain reaction liquid;
mixing the reaction solution with cation exchange resin for adsorption, and filtering after adsorption is finished to obtain filtrate;
the filtrate was concentrated and crystallized, and the crystals were collected and dried.
The embodiment of the invention has the beneficial effects that:
the embodiment of the invention provides a preparation method of high-quality zinc sulfate monohydrate, which comprises the steps of dispersing zinc oxide in water, adding concentrated sulfuric acid for reaction, and filtering after the reaction to obtain reaction liquid; and adsorbing the reaction solution by using cation exchange resin, filtering and crystallizing to obtain high-quality zinc sulfate monohydrate. The preparation method has the advantages of cheap and easily-obtained raw materials, simple and convenient operation and low requirement on equipment, and can quickly and efficiently prepare the zinc sulfate monohydrate. And the produced zinc sulfate monohydrate product has high purity which reaches over 99 percent, the quality meets the national standard, the content of alkali metal and alkaline earth metal is less than or equal to 0.5 percent, and the zinc sulfate monohydrate can be widely applied to the fields of food and medicine.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following is a detailed description of a high-quality zinc sulfate monohydrate and a preparation method thereof according to embodiments of the present invention.
The embodiment of the invention provides a preparation method of high-quality zinc sulfate monohydrate, which comprises the following steps:
s1, mixing zinc oxide with water to obtain a suspension;
s2, slowly adding concentrated sulfuric acid into the suspension for reaction under continuous stirring, and filtering after the reaction is finished to obtain reaction liquid;
s3, mixing the reaction solution with cation exchange resin for adsorption, and filtering after adsorption is finished to obtain filtrate;
s4, concentrating and crystallizing the filtrate, collecting crystals, and drying the crystals.
In the method, zinc oxide is dispersed in water and then reacts with concentrated sulfuric acid, so that the reaction process can be effectively controlled, and high-purity zinc sulfate can be quickly and efficiently obtained. And then the content of alkali metal and alkaline earth metal in the product can be effectively reduced by using cation exchange resin for adsorption, so that the high quality of the product is ensured.
Further, the mass ratio of zinc oxide to water is 1: 2.5 to 3.1. The mass ratio of the zinc oxide to the concentrated sulfuric acid is 1: 1.2 to 1.25. Under the proportion, the zinc oxide can obtain better dispersibility, and the efficiency and the safety of the reaction of the zinc oxide and concentrated sulfuric acid are ensured.
Further, the reaction of the suspension and concentrated sulfuric acid is carried out at room temperature by stirring, and the reaction time is 0.5-1.5 h. In the time range, the zinc oxide and the concentrated sulfuric acid can be fully reacted, and higher yield is obtained.
Further, the mass ratio of the zinc oxide to the cation adsorption resin is 1: 0.12 to 0.15. The mixed adsorption of the reaction solution and the cation exchange resin is carried out at room temperature by stirring, and the adsorption time is 2-4 h. Within the range, the cation adsorption resin can be fully contacted with zinc sulfate for adsorption, and the alkali metal and the alkaline earth metal contained in the cation adsorption resin can be effectively reduced.
Further, the filtrate is concentrated to 20-30% by volume. And precipitating crystals from the concentrated filtrate at 0-5 ℃. Under the conditions, the precipitation of zinc sulfate monohydrate crystals can be promoted, the residue of the zinc sulfate monohydrate crystals in the filtrate can be reduced, and the overall yield of the zinc sulfate monohydrate can be improved.
Further, the drying temperature of the crystal is 100-120 ℃, and the drying time is 2-4 h. Under the conditions, residual water in the zinc sulfate monohydrate can be effectively removed, and the product purity is improved.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of high-quality zinc sulfate monohydrate, which comprises the following steps:
s1, weighing 400 ml of distilled water, pouring the distilled water into a beaker, adding 130 g of zinc oxide, stirring, and uniformly dispersing to obtain a suspension;
and S2, taking 160 g of concentrated sulfuric acid, slowly dropwise adding the concentrated sulfuric acid into the suspension, stirring at room temperature for reaction for 1 hour, and filtering after the reaction is finished to obtain a reaction solution.
S3, mixing the reaction solution with 15 g of cation exchange resin, stirring and adsorbing for 3 hours at room temperature, and filtering after adsorption is finished to obtain filtrate.
S4, concentrating the volume of the filtrate to 30%, and separating out crystals at 0 ℃;
s5, filtering to collect crystals, and drying at 120 ℃ for 2 h to obtain high-quality zinc sulfate monohydrate (white solid, yield 87.9%, purity 99.3%, content of alkali metal and alkaline earth metal is less than 0.5%).
Example 2
The embodiment provides a preparation method of high-quality zinc sulfate monohydrate, which comprises the following steps:
s1, weighing 500 ml of distilled water, pouring the distilled water into a beaker, adding 200 g of zinc oxide, stirring, and uniformly dispersing to obtain a suspension;
and S2, taking 250 g of concentrated sulfuric acid, slowly dropwise adding the concentrated sulfuric acid into the suspension, stirring at room temperature for reaction for 1.5 hours, and filtering after the reaction is finished to obtain a reaction solution.
S3, mixing the reaction solution with 30 g of cation exchange resin, stirring and adsorbing for 2 hours at room temperature, and filtering after adsorption is finished to obtain filtrate.
S4, concentrating the volume of the filtrate to 20%, and separating out crystals at 5 ℃;
s5, filtering to collect crystals, and drying at 100 ℃ for 4 h to obtain high-quality zinc sulfate monohydrate (white solid, yield 85.3%, purity 99.1%, content of alkali metal and alkaline earth metal is less than 0.5%).
Example 3
The embodiment provides a preparation method of high-quality zinc sulfate monohydrate, which comprises the following steps:
s1, weighing 800 ml of distilled water, pouring the distilled water into a beaker, adding 300 g of zinc oxide, stirring, and uniformly dispersing to obtain a suspension;
and S2, taking 372 g of concentrated sulfuric acid, slowly dropwise adding the concentrated sulfuric acid into the suspension, stirring at room temperature for reaction for 1.5 hours, and filtering after the reaction is finished to obtain a reaction solution.
S3, mixing the reaction solution with 43 g of cation exchange resin, stirring and adsorbing for 4 hours at room temperature, and filtering after adsorption is finished to obtain filtrate.
S4, concentrating the volume of the filtrate to 20%, and separating out crystals at 0 ℃;
s5, filtering to collect crystals, and drying at 120 ℃ for 3 h to obtain high-quality zinc sulfate monohydrate (white solid, yield 86.1%, purity 99.3%, content of alkali metal and alkaline earth metal is less than 0.5%).
Example 4
The embodiment provides a preparation method of high-quality zinc sulfate monohydrate, which comprises the following steps:
s1, weighing 1000 ml of distilled water, pouring the distilled water into a beaker, adding 450 g of zinc oxide, stirring, and uniformly dispersing to obtain a suspension;
and S2, taking 560 g of concentrated sulfuric acid, slowly dropwise adding the concentrated sulfuric acid into the suspension, stirring at room temperature for reaction for 1.5 hours, and filtering after the reaction is finished to obtain a reaction solution.
S3, mixing the reaction solution with 65 g of cation exchange resin, stirring and adsorbing for 4 hours at room temperature, and filtering after adsorption is finished to obtain filtrate.
S4, concentrating the volume of the filtrate to 25%, and separating out crystals at 0 ℃;
s5, filtering to collect crystals, and drying at 120 ℃ for 1 h to obtain high-quality zinc sulfate monohydrate (white solid, yield 82.5%, purity 99.1%, content of alkali metal and alkaline earth metal is less than 0.5%).
Example 5
The embodiment provides a preparation method of high-quality zinc sulfate monohydrate, which comprises the following steps:
s1, weighing 2000 ml of distilled water, pouring the distilled water into a beaker, adding 680 g of zinc oxide, stirring, and uniformly dispersing to obtain a suspension;
and S2, taking 850 g of concentrated sulfuric acid, slowly dropwise adding the concentrated sulfuric acid into the suspension, stirring at room temperature for reaction for 1.5 hours, and filtering after the reaction is finished to obtain a reaction solution.
S3, mixing the reaction solution with 85 g of cation exchange resin, stirring and adsorbing for 2 hours at room temperature, and filtering after adsorption is finished to obtain filtrate.
S4, concentrating the volume of the filtrate to 30%, and separating out crystals at 0 ℃;
s5, filtering to collect crystals, and drying at 100 ℃ for 4 h to obtain high-quality zinc sulfate monohydrate (white solid, yield 78.3%, purity 99.0%, content of alkali metal and alkaline earth metal is less than 0.5%).
In summary, the embodiment of the present invention provides a preparation method of high quality zinc sulfate monohydrate, which includes dispersing zinc oxide in water, adding concentrated sulfuric acid for reaction, and filtering after reaction to obtain a reaction solution; and adsorbing the reaction solution by using cation exchange resin, filtering and crystallizing to obtain high-quality zinc sulfate monohydrate. The preparation method has the advantages of cheap and easily-obtained raw materials, simple and convenient operation and low requirement on equipment, and can quickly and efficiently prepare the zinc sulfate monohydrate. And the produced zinc sulfate monohydrate product has high purity which reaches over 99 percent, the quality meets the national standard, the content of alkali metal and alkaline earth metal is less than or equal to 0.5 percent, and the zinc sulfate monohydrate can be widely applied to the fields of food and medicine.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of high-quality zinc sulfate monohydrate is characterized by comprising the following steps:
mixing zinc oxide with water to obtain a suspension;
slowly adding concentrated sulfuric acid into the suspension for reaction under continuous stirring, and filtering after the reaction is finished to obtain a reaction solution;
mixing the reaction solution with cation exchange resin for adsorption, and filtering after adsorption is finished to obtain filtrate;
the filtrate was concentrated and crystallized, crystals were collected, and the crystals were dried.
2. The production method according to claim 1, wherein the mass ratio of the zinc oxide to the water is 1: 2.5 to 3.1.
3. The preparation method according to claim 1, wherein the mass ratio of the zinc oxide to the concentrated sulfuric acid is 1: 1.2 to 1.25.
4. The preparation method according to claim 2, wherein the reaction between the suspension and the concentrated sulfuric acid is carried out at room temperature with stirring for 0.5 to 1.5 hours.
5. The method according to claim 1, wherein the mass ratio of the zinc oxide to the cation adsorbent resin is 1: 0.12 to 0.15.
6. The preparation method according to claim 5, wherein the mixed adsorption of the reaction solution and the cation exchange resin is performed at room temperature with stirring, and the adsorption time is 2-4 h.
7. The method of claim 1, wherein the concentrating the filtrate is to concentrate the volume of the filtrate to 20% to 30%.
8. The method according to claim 7, wherein the filtrate after the concentration is crystallized, and the crystallization is performed at 0 to 5 ℃.
9. The preparation method according to claim 8, wherein the drying temperature of the crystal is 100 to 120 ℃ and the drying time is 2 to 4 hours.
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| EP0296148A1 (en) * | 1987-06-19 | 1988-12-21 | Chemson Polymer-Additive Gesellschaft M.B.H. | Process for the preparation of a mixture of zinc sulfate hydrate containing hexahydrate and heptahydrate which can be conserved |
| CN104229859A (en) * | 2014-10-10 | 2014-12-24 | 河南工信华鑫环保科技有限公司 | Method for removing iron impurities and gathering cupric ions in copper sulfate solution |
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| CN104556205A (en) * | 2014-12-31 | 2015-04-29 | 袁福堂 | Technical method for producing feed-grade zinc sulfate in environment-friendly manner by electrolytic zinc slag |
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