阅读说明：本技术 一种加热制备碱式氯化锌的方法 (Method for preparing basic zinc chloride by heating ) 是由 路东柱 蒋全通 马秀敏 王秀通 张�杰 段继周 黄彦良 侯保荣 于 2020-06-04 设计创作，主要内容包括：本发明涉及碱式氯化锌的制备方法,具体涉及一种利用氧化锌粉末和氯化铵粉末高温下加热制备碱式氯化锌的方法。利用氧化锌粉末和氯化铵粉末作为原料,在150℃-700℃下使粉末之间发生反应,获得碱式氯化锌。本发明所利用的原料为氯化铵及氧化锌粉末,原材料安全、环保、无污染、易保存,不采用有毒性、有腐蚀性且易吸湿的氯化锌作为原材料。(The invention relates to a preparation method of basic zinc chloride, in particular to a method for preparing basic zinc chloride by heating zinc oxide powder and ammonium chloride powder at a high temperature. Zinc oxide powder and ammonium chloride powder are used as raw materials, and the powder reacts at the temperature of 150-700 ℃ to obtain the basic zinc chloride. The raw materials used by the invention are ammonium chloride and zinc oxide powder, the raw materials are safe, environment-friendly, pollution-free and easy to store, and the zinc chloride which is toxic, corrosive and easy to absorb moisture is not used as the raw material.)

1. A method for preparing basic zinc chloride by heating is characterized in that: zinc oxide powder and ammonium chloride powder are used as raw materials, and the powder reacts at the temperature of 150-700 ℃ to obtain the basic zinc chloride.

2. The method of claim 1, wherein: and taking the zinc oxide powder and ammonium chloride powder as raw materials, covering the zinc oxide powder on the ammonium chloride powder, and carrying out heat preservation reaction at the temperature of 150-700 ℃ for 0.1-24 h to obtain the basic zinc chloride.

3. A method according to claim 1 or 2, characterized in that: the mass ratio of the zinc oxide powder to the ammonium chloride powder is 1:5-30: 1.

4. The method of claim 3, wherein: the mass ratio of the zinc oxide powder to the ammonium chloride powder is 1:1-10: 1.

5. A method according to claim 1 or 2, characterized in that: the reaction is carried out at 350-500 ℃ and the temperature is kept for 1-5 h.

6. A method according to claim 1 or 2, characterized in that: and after the heat preservation reaction, forcibly cooling or naturally cooling to room temperature to obtain the basic zinc chloride.

7. The method of claim 6, wherein: the product after the reaction is in a lump shape or larger particles and is rich in basic zinc chloride.

8. The method of claim 7, wherein: after the reaction, the product is subjected to centrifugal separation, washing, drying and crushing to obtain the high-purity basic zinc chloride.

Technical Field

The invention relates to a preparation method of basic zinc chloride, in particular to a method for preparing basic zinc chloride by heating zinc oxide powder and ammonium chloride powder at a high temperature.

Background

Zinc is one of important trace elements required by animals, and the zinc element plays an important role in maintaining the physiological functions of the animals and the like. Zinc source additives such as zinc oxide and zinc carbonate have the defect of low bioavailability. In comparison, the basic zinc chloride has higher bioavailability, better stability and more ideal effect of promoting the growth of animals.

The basic zinc chloride has the advantages of stable chemical property, small relative dosage, safety, no toxicity, high utilization efficiency, environmental protection, no pollution and the like, and is a good feed additive.

For example, patent ZL 200410023141.1 discloses a method for preparing basic zinc chloride by adding waste zinc into saturated zinc chloride solution, patent ZL 200610031714.4 discloses a method for preparing basic zinc chloride by adding zinc oxide into diluted hydrochloric acid solution, patent ZL 200910310420.9 discloses a method for preparing basic zinc chloride by adding ammonia water into zinc chloride solution, patent 200910310422.8 discloses a method for preparing basic zinc chloride by adding zinc chloride and zinc hydroxide slurry into water for reaction, patent ZL 201310075930.9 discloses a method for preparing basic zinc chloride by mixing calcium hydroxide suspension and zinc chloride solution, patent ZL201410334423.7 discloses a method for preparing basic zinc chloride by adding zinc powder into carbon tetrachloride solution and then adding distilled water, patent ZL201410585190.8 discloses a method for preparing basic zinc chloride by adding zinc chloride solution and ammonia water into hydrochloric acid solution dissolved with induction salt, patent ZL 201711252121.5 discloses a preparation method of basic zinc chloride using zinc chloride solution and ammonia water solution as main raw materials, wherein the above patents all use liquid as reaction raw material, the reaction systems are all liquid systems, and the related reactants such as hydrochloric acid, ammonia water, zinc chloride and the like have certain dangerousness, toxicity and volatility. The product generated by liquid reaction precipitation also needs to be washed, dried and the like. And a more concise, effective, economic and rapid preparation mode of basic zinc chloride, especially a preparation mode of basic zinc chloride which does not relate to liquid raw materials, is sought.

Disclosure of Invention

The invention aims to provide a preparation method of basic zinc chloride, which adopts solid powder as a raw material and does not relate to solution reaction, so that the preparation of the basic zinc chloride gets rid of the dependence on a liquid reaction system, and more choices are provided for efficiently, excellently and cheaply preparing the basic zinc chloride.

In order to achieve the purpose, the technical scheme of the invention is as follows:

a method for preparing basic zinc chloride by heating utilizes zinc oxide powder and ammonium chloride solid powder as raw materials, and makes the powder react at 150-700 ℃ to obtain the basic zinc chloride.

Preferably, the zinc oxide powder and the ammonium chloride powder are used as raw materials, the zinc oxide powder covers the ammonium chloride powder, and the basic zinc chloride is obtained after heat preservation reaction for 0.1-24 hours at the temperature of 150-700 ℃ (the reaction temperature is the heating reaction temperature of the ammonium chloride powder and the zinc oxide powder, so that the ammonium chloride powder is decomposed, and simultaneously the sublimation temperature of the zinc chloride powder is lower).

The mass ratio of the zinc oxide powder to the ammonium chloride powder is 1:5-30: 1.

The mass ratio of the zinc oxide powder to the ammonium chloride powder is 1:1-10: 1; it is further preferred that the ratio of the amount of zinc oxide to ammonium chloride species is about 5: 2.

The reaction is carried out at 350-500 ℃, and in order to fully carry out the reaction and improve the preparation efficiency, the heating time can be 1-5 h.

And after the heat preservation reaction, obtaining the basic zinc chloride by forced cooling or natural cooling. After the heating is finished, the crucible and the powder in the crucible need to be cooled to room temperature; in order to reduce the cost, the air cooling mode can be adopted, and the air cooling mode can be naturally cooled to the room temperature under the atmosphere.

The invention has the advantages that:

1. the invention obtains high-quality and high-yield basic zinc chloride by utilizing the modes that ammonium chloride powder and zinc oxide powder are decomposed in a heating state through ammonium chloride, and chemical reactions occur between the powder and between the powder and gas.

2. The raw materials used by the invention are ammonium chloride and zinc oxide powder, the raw materials are safe, environment-friendly, pollution-free and easy to store, the zinc chloride which is toxic, corrosive and easy to absorb moisture is not used as the raw material, and acid solution or alkali solution such as hydrochloric acid, ammonia water and the like is not required to be introduced. No inducing salt is needed, so that impurity elements brought by the inducing salt are avoided.

3. Compared with a liquid reaction method which needs to prepare various volatile and corrosive solutions, the method has the advantages of simple required equipment, simple procedure, safety, environmental protection, no pollution, convenient operation and easy realization, and does not relate to dilution, blending, mixing, pH adjustment and the like of liquid raw materials.

4. The method completely decomposes the ammonium chloride at a higher temperature, the ammonia escapes, the rest elements are basic zinc chloride composition elements, other impurity elements are not introduced, the obtained basic zinc chloride is pure, and the utilization rate of zinc elements is high.

Drawings

FIG. 1 is a schematic diagram of a preparation method of basic zinc chloride provided by the invention.

FIG. 2 is a scanning electron micrograph of zinc oxychloride obtained in example 1 of the present invention.

Detailed Description

The following examples are presented to further illustrate embodiments of the present invention, and it should be understood that the embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the invention.

Unless otherwise specified, the reagents used in the following examples are commercially available from normal sources.

Example 1

Firstly, 5g of zinc oxide powder and 1g of ammonium chloride powder are selected as raw materials.

Secondly, placing ammonium chloride powder at the bottom of the crucible, covering zinc oxide powder on the ammonium chloride powder, and placing the mixture in a heating furnace to heat and preserve heat at 400 ℃;

thirdly, heating the crucible containing the powder at 400 ℃ and keeping the temperature for 2 hours;

fourthly, after the heat preservation is finished, the crucible containing the powder is placed in the air to be naturally cooled;

fifthly, after cooling to room temperature, removing the residual powder, and obtaining the block-shaped basic zinc chloride at the bottom of the crucible. The scanning electron microscope photograph of the crushed zinc oxychloride particles is shown in fig. 2.

As can be seen from FIG. 2, the basic zinc chloride particles have irregular shapes, loose and porous surfaces and are covered with microscopic layers. .

Sixthly, carrying out centrifugal separation, water washing, drying, crushing and packaging on the block basic zinc chloride. Removing the zinc oxide powder possibly in excess by using a centrifugal separator; washing the obtained block-shaped product in water, and further purifying the basic zinc chloride by utilizing the characteristics that the zinc oxide is easily dissolved in the water and the basic zinc chloride is not easily dissolved in the water; drying the water-insoluble substances at low temperature after washing, wherein the drying temperature can be controlled at 50 ℃; crushing the dried product into finer powder by a mechanical method; and packaging the final product.

Example 2

The preparation method of this example is the same as example 1, except that: in the first step, 5g of zinc oxide powder and 2g of ammonium chloride powder are selected as raw materials.

Example 3

The preparation method of this example is the same as example 1, except that: in the second step, the heating furnace heats the mixture to the temperature of 430 ℃.

Example 4

The preparation method of this example is the same as example 1, except that: the heating and heat preservation time in the third step is 3 h.

Example 5

The preparation method of this example is the same as example 1, except that: and in the fourth step, forced ventilation cooling is carried out by adopting a fan.

Example 6

The preparation method of this example is the same as example 1, except that: and fifthly, stirring the substances in the crucible by adopting stirring and other modes before cooling to the room temperature, and preventing the basic zinc chloride from being attached to the crucible.

Example 7

The preparation method of this example is the same as example 1, except that: and step six, omitting operations of centrifugal separation, water washing, drying, crushing and packaging according to specific requirements.

Example 8

The preparation method of this example is the same as example 1, except that: and step six, omitting operations of centrifugal separation, water washing and drying according to specific requirements, and only carrying out crushing and packaging.

The reactants in the above embodiments do not relate to toxic and harmful substances such as hydrochloric acid, ammonia water, zinc chloride and the like, only solid zinc oxide powder and ammonium chloride powder are used as raw materials, the raw materials are green, healthy, environment-friendly and pollution-free, meanwhile, the ammonium chloride powder in the raw materials is decomposed in the heating process, ammonia gas escapes, the remaining elements such as Zn, Cl, O, H and the like are basic zinc chloride forming substances, and the reaction product does not contain impurity elements; meanwhile, the solid powder reactant occupies small volume compared with various aqueous solutions, the whole reaction process can be completed by only adopting one crucible, the space utilization rate is greatly improved, and precious fresh water resources are saved; the obtained basic zinc chloride can be used as a food additive to promote animal growth, and the production and preparation process of the basic zinc chloride is simplified.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.