阅读说明：本技术 一种氧化锌的生产方法 (Production method of zinc oxide ) 是由 赵尹 蒋航宇 王璐 刘宇豪 董飘平 于 2021-09-10 设计创作，主要内容包括：本发明公开了一种氧化锌的生产方法,氧化锌矿加浸出剂进行浸出,浸出后过滤得到浸出液及浸出渣(2)将所述浸出液加沉淀剂进行氧化锌析出,陈化后过滤氧化锌析出物,得到氧化锌产品和滤液；(3)将所述滤液进行低温蒸馏回收沉淀剂。本发明采用上述结构的一种氧化锌的生产方法,流程短,易于控制,并且可以根据需要控制反应参数,以得到不同粒径的氧化锌颗粒。(The invention discloses a production method of zinc oxide, which comprises the steps of adding a leaching agent into zinc oxide ores for leaching, filtering the leached zinc ores to obtain a leaching solution and leaching residues (2), adding a precipitator into the leaching solution for zinc oxide precipitation, and filtering zinc oxide precipitates after aging to obtain a zinc oxide product and a filtrate; (3) and distilling the filtrate at low temperature to recover the precipitant. The production method of zinc oxide with the structure is short in flow and easy to control, and reaction parameters can be controlled according to needs to obtain zinc oxide particles with different particle sizes.)

1. A production method of zinc oxide is characterized by comprising the following steps:

(1) adding a leaching agent into the zinc oxide ore for leaching, and filtering after leaching to obtain a leaching solution and leaching residues

(2) Adding a precipitator into the leachate to separate out zinc oxide, and filtering the zinc oxide precipitate after aging to obtain a zinc oxide product and a filtrate;

(3) and distilling the filtrate at low temperature to recover the precipitant.

2. The method for producing zinc oxide according to claim 1, wherein: in the leaching process in the step (1), the concentration of the leaching agent is 4-8 mol/L, and the leaching agent is one or more of alkaline leaching agents such as NaOH, KOH and LiOH.

3. The method for producing zinc oxide according to claim 1, wherein: in the step (1), the leaching conditions are that the leaching temperature is 10-100 ℃, and the leaching stirring speed is 100-500 rpm.

4. The method for producing zinc oxide according to claim 1, wherein: in the step (2), the precipitant is one or more of methanol, 1-propanol, 2-propanol, and the like.

5. The method for producing zinc oxide according to claim 1, wherein: in the step (2), the ratio of the precipitator to the leaching solution is 0.1-10.

6. The method for producing zinc oxide according to claim 1, wherein: in the step (2), the temperature of the zinc oxide is-10-70 ℃.

7. The method for producing zinc oxide according to claim 1, wherein: in the step (2), zinc oxide crystals are added in advance for crystallization in the zinc oxide precipitation process, so as to obtain zinc oxide particles with different sizes and shapes.

8. The method for producing zinc oxide according to claim 1, wherein: in the step (3), in the low-temperature distillation process, the distillation temperature is 60-80 ℃.

9. The method for producing zinc oxide according to claim 1, wherein: the filtering equipment is one or more of a filter press, a thickener, a centrifuge and the like.

10. The method for producing zinc oxide according to claim 1, wherein: the distillation apparatus includes, but is not limited to, a distillation column, vacuum distillation, vacuum membrane distillation.

Technical Field

The invention relates to the technical field of wet metallurgy, in particular to a production method of zinc oxide.

Background

Hydrometallurgical processes are more environmentally friendly and economically attractive for the production of zinc oxide, especially on a small scale. There are many traditional zinc oxide production methods, including precipitation method, combustion method, water (solvent) thermal method, etc., and all zinc oxide production processes generate white precipitate (such as Zn) as intermediate product₅(CO₃)₂(OH)₆Etc.) and then regenerated to oxidationThe invention adopts an alkaline precipitation method to produce zinc oxide, does not need to generate intermediate products, and can directly crystallize from the leaching solution to obtain a zinc oxide product.

Disclosure of Invention

The invention aims to provide a production method of zinc oxide, which has simple operation, short flow and easy control, and can control reaction parameters according to requirements to obtain zinc oxide particles with different particle sizes.

In order to achieve the above object, the present invention provides a method for producing zinc oxide, comprising the steps of:

(1) adding a leaching agent into the zinc oxide ore for leaching, and filtering after leaching to obtain a leaching solution and leaching residues

(2) Adding a precipitator into the leachate to separate out zinc oxide, and filtering the zinc oxide precipitate after aging to obtain a zinc oxide product and a filtrate;

(3) and distilling the filtrate at low temperature to recover the precipitant.

Preferably, in the leaching process in step (1), the concentration of the leaching agent is 4-8 mol/L, and the leaching agent is one or more of alkaline leaching agents such as NaOH, KOH and LiOH.

Preferably, in the step (1), the leaching condition is that the leaching temperature is 10-100 ℃, and the leaching stirring speed is 100-500 rpm.

Preferably, in step (2), the precipitating agent is one or more of methanol, 1-propanol, 2-propanol, etc.

Preferably, in the step (2), the ratio of the precipitant to the leachate is 0.1-10.

Preferably, in the step (2), the temperature of the zinc oxide precipitation is-10 to 70 ℃.

Preferably, in the step (2), zinc oxide crystals are added in advance for crystallization in the zinc oxide precipitation process, so as to obtain zinc oxide particles with different sizes and shapes.

Preferably, in the step (3), the distillation temperature in the low-temperature distillation process is 60-80 ℃.

Preferably, the filtering device is one or more of a filter press, a thickener, a centrifuge, and the like.

Preferably, the distillation apparatus includes, but is not limited to, a distillation column, vacuum distillation, vacuum membrane distillation.

The invention has the beneficial effects that:

(1) compared with the original zinc oxide production flow, the method directly uses the leaching solution to produce the zinc oxide, does not form intermediate products such as zinc hydroxide and zinc carbonate in the traditional zinc oxide production process, and shortens the production flow;

(2) the precipitator used in the zinc oxide production process is non-toxic and harmless, is a green precipitator, is cheap and easy to obtain, and has industrial applicability;

(3) the zinc oxide used in the invention has mild production conditions, does not need high temperature and additives, and is a zinc oxide production process with low cost and short flow.

The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.

Drawings

FIG. 1 is a comparison of XRD analysis of zinc oxide and analytically pure zinc oxide from a process for producing zinc oxide according to the present invention;

FIG. 2 is a process flow diagram of a method for producing zinc oxide according to the present invention.

Detailed Description

The present invention will be further described with reference to examples, in which various chemicals and reagents are commercially available unless otherwise specified.

Example 1

(1) Weighing 7g of zinc oxide ore, adding 100ml of 8mol/L sodium hydroxide solution, placing the zinc oxide ore into a beaker, keeping the stirring speed at 200rpm, and leaching in a water bath at 60 ℃; leaching for 4 hours, and filtering to obtain a leaching solution;

(2) keeping the stirring speed and the water bath temperature, slowly adding 100ml of precipitator into the leaching solution, wherein the precipitator is prepared by mixing methanol and isopropanol according to the volume ratio of 2:3, controlling the adding time to be 1h, aging for 0.5h after the precipitator is added, and filtering the precipitate to obtain a zinc oxide product and a filtrate; the yield of zinc oxide is 96%, and the particle size of zinc oxide particles is 10 μm;

(3) and (3) putting the filtrate into a distillation flask, distilling and condensing at 80 ℃ to recover a precipitator, and repeating the step (1) to carry out circulating leaching, wherein the rest is a sodium hydroxide solution containing a small amount of zinc (<3 g/L).

Example 2

(1) Weighing 10g of zinc oxide ore, adding 100ml of 7mol/L sodium hydroxide solution, placing the mixture into a beaker, keeping the stirring speed at 200rpm, and leaching in a water bath at 60 ℃; leaching for 4 hours, and filtering to obtain a leaching solution;

(2) keeping stirring speed and water bath temperature, slowly adding 200ml of precipitant into the leachate, mixing the precipitant with methanol and 2-propanol at a volume ratio of 1:2, controlling the adding time to be 2h, aging for 0.5h after adding the precipitant, and filtering the precipitate to obtain zinc oxide product and filtrate; the yield of zinc oxide is 98%, and the particle size of zinc oxide particles is 15 μm;

(3) and (3) putting the filtrate into a distillation flask, distilling and condensing at 80 ℃ to recover a precipitator, and repeating the step (1) to carry out circulating leaching, wherein the rest is a sodium hydroxide solution containing a small amount of zinc (<1 g/L).

Example 3

(1) Weighing 5g of zinc oxide ore, adding 100ml of 6mol/L sodium hydroxide solution, placing the mixture in a beaker, keeping the stirring rotation speed at 200rpm, leaching in a water bath at 50 ℃ for 2 hours to obtain a leaching solution;

(2) keeping the stirring speed and the water bath temperature, slowly adding 100ml of precipitator into the leaching solution, wherein the precipitator is prepared by mixing methanol and 2-propanol according to the volume ratio of 2: 1), and controlling the adding time to be 4 h; after adding the precipitator, aging for 1h, and filtering precipitates to obtain a zinc oxide product and a filtrate; the yield of zinc oxide is 97%, and the particle size of zinc oxide particles is 20 μm;

(3) and (3) putting the filtrate into a distillation flask, distilling and condensing at 80 ℃ to recover a precipitator, and repeating the step (1) to carry out circulating leaching, wherein the rest is a sodium hydroxide solution containing a small amount of zinc (<3 g/L).

Example 4

(1) Weighing 15g of zinc oxide ore, adding 100ml of 8mol/L sodium hydroxide solution, placing the zinc oxide ore into a beaker, keeping the stirring speed at 200rpm, and leaching in 70 ℃ water bath; leaching for 2 hours to obtain a leaching solution;

(2) cooling the leaching solution to normal temperature, stirring at 100rpm, slowly adding 150ml of precipitator into the leaching solution, wherein the precipitator is prepared by mixing isopropanol and 2-propanol according to a volume ratio of 1:1, and the adding time is controlled to be 3 h; after adding the precipitator, aging for 2 hours, and filtering precipitates to obtain a zinc oxide product and a filtrate; the yield of zinc oxide is 97%, and the particle size of zinc oxide particles is 20 μm;

(3) and (3) putting the filtrate into a distillation flask, distilling and condensing at 80 ℃ to recover a precipitator, and repeating the step (1) to carry out circulating leaching, wherein the rest is a sodium hydroxide solution containing a small amount of zinc (<3 g/L).

Example 5

(1) Weighing 6g of zinc oxide ore, adding 100ml of sodium hydroxide solution with the concentration of 4mol/L, placing the zinc oxide ore into a beaker, keeping the stirring speed at 200rpm, and leaching in a water bath at 30 ℃; leaching for 3h to obtain a leaching solution;

(2) keeping the stirring speed and the water bath temperature, slowly adding 150ml of precipitator into the leaching solution, wherein the precipitator is prepared by mixing methanol and 2-propanol according to the volume ratio of 2:1, and the adding time is controlled to be 3 hours; after adding the precipitator, aging for 2 hours, and filtering precipitates to obtain a zinc oxide product and a filtrate; the yield of zinc oxide is 96%, and the particle size of zinc oxide particles is 16 μm;

(3) and (3) putting the filtrate into a distillation flask, distilling and condensing at 80 ℃ to recover a precipitator, and repeating the step (1) to carry out circulating leaching, wherein the rest is a sodium hydroxide solution containing a small amount of zinc (<3 g/L).

Example 6

(1) Weighing 6g of zinc oxide, adding 100ml of sodium hydroxide solution with the concentration of 4mol/L, placing the zinc oxide in a beaker, keeping the stirring speed at 200rpm, and leaching in a water bath at 30 ℃; leaching for 3h to obtain a leaching solution;

(2) keeping the stirring speed and the water bath temperature, firstly adding zinc oxide seed crystals with the concentration of 30g/L into the leaching solution, then slowly adding 150ml of precipitator, wherein the precipitator is prepared by mixing methanol and 2-propanol according to the volume ratio of 2:1, and the adding time is controlled to be 3 hours; after adding the precipitator, aging for 2 hours, and filtering precipitates to obtain a zinc oxide product and a filtrate; the yield of zinc oxide was 97%, and the particle size of the zinc oxide particles was 50 μm;

(4) and (3) putting the filtrate into a distillation flask, distilling and condensing at 80 ℃ to recover a precipitator, and repeating the step (1) to carry out circulating leaching, wherein the rest is a sodium hydroxide solution containing a small amount of zinc (<3 g/L).

Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.