阅读说明：本技术 一种利用磷尾矿制取高品质碳酸钙和氢氧化镁的方法 (Method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings ) 是由 李万清 肖林波 田承涛 方超 廖秋实 周玲玲 于 2021-01-11 设计创作，主要内容包括：一种利用磷尾矿制取高品质碳酸钙和氢氧化镁的方法,包括如下过程：将磷尾矿、盐酸按比例加入分解槽,在分解槽内充分混合反应,反应料浆进行固液分离,分离出含氯化钙和氯化镁的滤液和固体废渣为酸不溶物。含氯化钙和氯化镁的滤液加入碳酸氢铵反应结晶,生成含杂质的碳酸钙。结晶料浆进行固液分离,分离出含杂质的碳酸钙,滤液仍为含氯化钙和氯化镁的滤液。滤液加入碳酸氢铵反应结晶,生成高品质的碳酸钙。结晶料浆进行固液分离,分离出高品质的碳酸钙,滤液为含氯化镁的滤液。氯化镁滤液通入气氨(液氨或氨水),得到氢氧化镁沉淀和氯化铵溶液。经固液分离得到氯化铵溶液和氢氧化镁固体。氯化铵溶液经浓缩、结晶得到氯化铵晶体。(A method for preparing high-quality calcium carbonate and magnesium hydroxide by utilizing phosphate tailings comprises the following steps: adding phosphate tailings and hydrochloric acid into a decomposition tank in proportion, fully mixing and reacting in the decomposition tank, carrying out solid-liquid separation on reaction slurry, and separating filtrate containing calcium chloride and magnesium chloride and solid waste residues to obtain acid-insoluble substances. Adding ammonium bicarbonate into the filtrate containing calcium chloride and magnesium chloride for reaction and crystallization to generate calcium carbonate containing impurities. And (4) carrying out solid-liquid separation on the crystallized slurry to separate calcium carbonate containing impurities, wherein the filtrate is the filtrate containing calcium chloride and magnesium chloride. Adding ammonium bicarbonate into the filtrate to react and crystallize to produce high-quality calcium carbonate. And carrying out solid-liquid separation on the crystallized slurry to separate high-quality calcium carbonate, wherein the filtrate is the filtrate containing magnesium chloride. Introducing gas ammonia (liquid ammonia or ammonia water) into the magnesium chloride filtrate to obtain magnesium hydroxide precipitate and ammonium chloride solution. And performing solid-liquid separation to obtain an ammonium chloride solution and a magnesium hydroxide solid. And concentrating and crystallizing the ammonium chloride solution to obtain ammonium chloride crystals.)

1. A method for preparing high-quality calcium carbonate and magnesium hydroxide by utilizing phosphate tailings is characterized by comprising the following steps:

step 1, adding phosphorus tailings and hydrochloric acid or sulfuric acid or nitric acid into a decomposition tank according to a ratio, fully mixing and reacting in the decomposition tank, controlling the reaction temperature to be 9-42 ℃, wherein the reaction time is more than or equal to 30 minutes, and the main effective components of the phosphorus tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state;

step 2, carrying out solid-liquid separation on the reaction slurry obtained in the step 1 to separate out a solution containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid waste residues which are acid insoluble substances;

step 3, adding the solution containing calcium chloride and magnesium chloride obtained in the step 2 into ammonium bicarbonate according to a proportion for reaction and crystallization, and controlling the reaction pH value, the reaction temperature and the reaction time to generate calcium carbonate containing impurities;

step 4, carrying out solid-liquid separation on the crystallized slurry obtained in the step 3, wherein the separated filter cake is calcium carbonate containing impurities, the filtrate is still a mixed solution containing calcium chloride and magnesium chloride, and washing the filter cake with water to obtain calcium carbonate containing impurities;

step 5, adding ammonium bicarbonate into the solution obtained in the step 4 according to a proportion, reacting and crystallizing, and controlling the reaction pH value, the reaction temperature and the reaction time to generate high-quality calcium carbonate;

step 6, carrying out solid-liquid separation on the crystallized slurry obtained in the step 5, wherein the separated filter cake is high-quality calcium carbonate, and the filtrate is a solution containing magnesium chloride;

step 7, introducing gas ammonia or liquid ammonia or ammonia water into the magnesium chloride-containing solution obtained in the step 6, controlling a proper pH value to obtain magnesium hydroxide precipitate and an ammonium chloride solution, performing solid-liquid separation to obtain an ammonium chloride solution and a magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide;

and 8, concentrating and crystallizing the ammonium chloride solution obtained in the step 7 to obtain ammonium chloride crystals.

2. The method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings as claimed in claim 1, which is characterized in that: and 3, the dosage of the ammonium bicarbonate in the step 3 is based on the pH value of the solution after the reaction, the pH value is controlled to be 2.5-5.4, the reaction temperature is 9-40 ℃, and the reaction time is more than or equal to 30 minutes.

3. The method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings as claimed in claim 1, which is characterized in that: and 5, the dosage of the ammonium bicarbonate in the step 5 is based on the pH value of the solution after the reaction, the pH value is controlled to be 4.5-6.5, the reaction temperature is 35-40 ℃, and the reaction time is more than or equal to 30 minutes.

4. The method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings as claimed in claim 2, which is characterized in that: and 3, the amount of ammonium bicarbonate in the step 3 is 4.8-5.3 according to the pH value of the solution after reaction.

5. The method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings as claimed in claim 3, which is characterized in that: and 5, the amount of ammonium bicarbonate in the step 5 is 5.8-6.4 according to the pH value of the solution after reaction.

6. The method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings as claimed in claim 1, which is characterized in that: the pH value in the step 7 is 7.5-10.0.

7. The method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings as claimed in claim 1, which is characterized in that: the acid-insoluble substance in the step 2 can be used as a raw material for firing cement; the calcium carbonate containing impurities in the step 4 is used as a filling material for producing the compound fertilizer; the ammonium chloride crystal in the step 8 is ammonium chloride with high purity, and can be used as a raw material of a full water-soluble fertilizer or a compound fertilizer.

8. The method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings as claimed in claim 1, which is characterized in that: and (5) enabling the solution in the step (4) in the step (5) to enter a cyclone, rotating at a speed of more than 7 m/min for 5-10 minutes, discharging the solution out of the cyclone, and mixing and reacting the solution with ammonium bicarbonate.

9. The method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings as claimed in claim 1, which is characterized in that: in the step 7, the magnesium chloride-containing solution in the step 6 and liquid ammonia are mixed in a cross flow mode.

Technical Field

The invention belongs to the technical field of chemical industry, and relates to a method for preparing high-quality calcium carbonate and magnesium hydroxide by utilizing phosphate tailings, in particular to a method for preparing high-quality calcium carbonate and magnesium hydroxide by decomposing phosphate tailings by utilizing hydrochloric acid to obtain calcium chloride and magnesium chloride and combining ammonium bicarbonate and ammonia.

Background

The reserve resources of phosphorite in China are relatively rich, but most phosphorite is of medium and low grade, and most phosphorite belongs to difficult ore dressing. As a big country of agriculture, phosphorite resources are largely used in the production of agricultural chemical fertilizers, and the phosphorus resources are shifted from rich mining to medium-low-grade lean mining, so that a large amount of phosphorus tailings are generated. The accumulation of the phosphate tailings not only causes resource waste, but also causes serious environmental pollution. The proportion of the effective elements of calcium, magnesium and phosphorus in the phosphate tailings is still large, and recycling the phosphate tailings and changing waste into valuable are always hot points of research in the industry.

The magnesium hydroxide product is mainly in the form of slurry, paste and powder, can be divided into nano-scale, fibrous, flame-retardant and environment-friendly magnesium hydroxide according to the functions, and is widely applied to important inorganic chemicals such as water treatment, flue gas desulfurization, inorganic flame retardants and the like. The high-quality calcium carbonate can be used as a raw material for producing potassium dihydrogen phosphate by our company, and a complete industrial chain is formed. Hydrochloric acid is a byproduct of the compound fertilizer, and has low quality and excessive productivity, thereby seriously restricting the productivity of the compound fertilizer. The hydrochloric acid is used for decomposing the phosphate tailings, so that the phosphate tailings can be utilized, and the surplus capacity of the hydrochloric acid is decomposed.

Disclosure of Invention

The invention aims to solve the problems and provides a method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings, which can produce high-quality magnesium hydroxide and calcium carbonate by using industrial wastes and low-price raw materials.

The technical scheme adopted by the invention is as follows: a method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings comprises the following specific steps:

a method for preparing high-quality calcium carbonate and magnesium hydroxide by using phosphate tailings;

step 1, adding phosphorus tailings and hydrochloric acid or sulfuric acid or nitric acid into a decomposition tank according to a ratio, fully mixing and reacting in the decomposition tank, controlling the reaction temperature to be 9-42 ℃, wherein the reaction time is more than or equal to 30 minutes, and the main effective components of the phosphorus tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state;

step 2, carrying out solid-liquid separation on the reaction slurry obtained in the step 1 to separate out a solution containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid waste residues which are acid insoluble substances;

step 3, adding the solution containing calcium chloride and magnesium chloride obtained in the step 2 into ammonium bicarbonate according to a proportion for reaction and crystallization, and controlling the reaction pH value, the reaction temperature and the reaction time to generate calcium carbonate containing impurities;

step 4, carrying out solid-liquid separation on the crystallized slurry obtained in the step 3, wherein the separated filter cake is calcium carbonate containing impurities, the filtrate is still a mixed solution containing calcium chloride and magnesium chloride, and washing the filter cake with water to obtain calcium carbonate containing impurities;

step 5, adding ammonium bicarbonate into the solution obtained in the step 4 according to a proportion, reacting and crystallizing, and controlling the reaction pH value, the reaction temperature and the reaction time to generate high-quality calcium carbonate;

step 6, carrying out solid-liquid separation on the crystallized slurry obtained in the step 5, wherein the separated filter cake is high-quality calcium carbonate, and the filtrate is a solution containing magnesium chloride;

step 7, introducing gas ammonia or liquid ammonia or ammonia water into the magnesium chloride-containing solution obtained in the step 6, controlling a proper pH value to obtain magnesium hydroxide precipitate and an ammonium chloride solution, performing solid-liquid separation to obtain an ammonium chloride solution and a magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide;

and 8, concentrating and crystallizing the ammonium chloride solution obtained in the step 7 to obtain ammonium chloride crystals.

Further, the amount of ammonium bicarbonate in the step (3) is based on the pH value of the solution after the reaction, the pH value is controlled to be 2.5-5.4, the reaction temperature is 9-40 ℃, and the reaction time is not less than 30 minutes.

Further, the amount of ammonium bicarbonate in the step (5) is based on the pH value of the solution after the reaction, the pH value is controlled to be 4.5-6.5, the reaction temperature is 35-40 ℃, and the reaction time is not less than 30 minutes.

Further, the amount of ammonium bicarbonate in the step (3) is 4.8-5.3 based on the pH value of the solution after the reaction.

Further, the amount of ammonium bicarbonate in the step (5) is 5.8-6.4 based on the pH value of the solution after the reaction.

Further, the pH value in the step (7) is 7.5-10.0.

Further, the acid-insoluble substance in the step (2) can be used as a raw material for firing cement; the calcium carbonate containing impurities in the step (4) is used as a filling material for producing the compound fertilizer; the ammonium chloride crystal in the step (8) is ammonium chloride with high purity and can be used as a raw material of a full water-soluble fertilizer or a compound fertilizer.

And (3) further, the solution in the step (4) in the step (5) enters a cyclone, rotates at a speed of more than 7 m/min for 5-10 minutes, is discharged out of the cyclone, and is mixed with ammonium bicarbonate for reaction.

Further, in the step 7, the magnesium chloride-containing solution in the step 6 and liquid ammonia are mixed in a cross flow mode.

The invention has the following beneficial effects:

1. the invention aims to provide a method for comprehensively utilizing a large amount of stacked phosphorus tailings and hydrochloric acid as a byproduct of compound fertilizer by using hydrochloric acid and phosphorus tailings as raw materials, successfully solving the problem that the hydrochloric acid and the phosphorus tailings cannot be treated, changing waste into valuable, and reducing the environmental protection pressure and the safety problem of phosphorus tailings stacking.

2. The process belongs to full resource utilization and accords with the concept of green chemical industry.

3. The invention has simple production process, convenient operation, low production cost and good economic benefit.

Drawings

FIG. 1 is a schematic process flow diagram of the present invention.

Detailed Description

The present invention will be further described with reference to the following embodiments and the accompanying drawings, but the embodiments are not intended to limit the present invention.

Implementation 1:

adding phosphate tailings (the main effective components of the phosphate tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state) and hydrochloric acid into a decomposition tank, and reacting for 30 minutes. And (3) carrying out solid-liquid separation on the reaction slurry, separating filtrate containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid which is an acid insoluble substance.

Adding ammonium bicarbonate into filtrate containing calcium chloride and magnesium chloride, reacting and crystallizing, controlling the pH value to be 4.8, controlling the reaction time to be 30 minutes, controlling the reaction temperature to be 9-42 ℃, heating when the temperature is lower than 9 ℃ in winter, and cooling when the temperature is higher than 42 ℃ in summer to obtain the calcium carbonate containing impurities. And (3) carrying out solid-liquid separation on the slurry containing calcium carbonate, washing the filter cake to obtain calcium carbonate (1), continuously adding ammonium bicarbonate into the filtrate for reaction and crystallization, controlling the pH value to be 5.8, and controlling the reaction time to be 35 minutes to obtain the high-quality calcium carbonate. And (3) carrying out solid-liquid separation on the slurry containing the calcium carbonate, and washing the filter cake to obtain calcium carbonate (2), wherein the filtrate is the filtrate containing magnesium chloride.

And introducing ammonia gas into the magnesium chloride filtrate, and controlling the pH value to be 8 to obtain magnesium hydroxide precipitate and an ammonium chloride solution. And (3) carrying out solid-liquid separation to obtain magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide.

And concentrating and crystallizing the separated ammonium chloride solution to obtain magnesium ammonium chloride crystals.

Calcium carbonate (1) obtained: purity: 50 percent;

calcium carbonate (2): purity: 96.2 percent;

magnesium hydroxide: purity: 97 percent;

ammonium chloride crystals: purity: 97 percent.

Implementation 2:

adding phosphate tailings (the main effective components of the phosphate tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state) and hydrochloric acid into a decomposition tank, and reacting for 35 minutes. And (3) carrying out solid-liquid separation on the reaction slurry, separating filtrate containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid which is an acid insoluble substance.

Adding ammonium bicarbonate into filtrate containing calcium chloride and magnesium chloride for reaction and crystallization, controlling the pH value to be 5, controlling the reaction time to be 35 minutes, controlling the reaction temperature to be 9-42 ℃, heating when the temperature is lower than 9 ℃ in winter, and cooling when the temperature is higher than 42 ℃ in summer to obtain the calcium carbonate containing impurities. And (3) carrying out solid-liquid separation on the slurry containing calcium carbonate, washing the filter cake with water to obtain calcium carbonate (1), continuously adding ammonium bicarbonate into the filtrate for reaction and crystallization, controlling the pH value to be 6, and controlling the reaction time to be 30 minutes to obtain the high-quality calcium carbonate. And (3) carrying out solid-liquid separation on the slurry containing the calcium carbonate, and washing the filter cake to obtain calcium carbonate (2), wherein the filtrate is the filtrate containing magnesium chloride.

And introducing ammonia gas into the magnesium chloride filtrate, and controlling the pH value to be 8.5 to obtain magnesium hydroxide precipitate and an ammonium chloride solution. And (3) carrying out solid-liquid separation to obtain magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide.

And concentrating and crystallizing the separated ammonium chloride solution to obtain magnesium ammonium chloride crystals.

Calcium carbonate (1) obtained: purity: 55 percent;

calcium carbonate (2): purity: 96.6 percent;

magnesium hydroxide: purity: 97.1 percent;

ammonium chloride crystals: purity: 97 percent.

Implementation 3:

adding phosphate tailings (the main effective components of the phosphate tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state) and hydrochloric acid into a decomposition tank, and reacting for 40 minutes. And (3) carrying out solid-liquid separation on the reaction slurry, separating filtrate containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid which is an acid insoluble substance.

Adding ammonium bicarbonate into the filtrate containing calcium chloride and magnesium chloride, reacting and crystallizing, controlling the pH value to be 5.2, and controlling the reaction time to be 40 minutes to obtain the calcium carbonate containing impurities. And (3) carrying out solid-liquid separation on the slurry containing calcium carbonate, washing the filter cake to obtain calcium carbonate (1), continuously adding ammonium bicarbonate into the filtrate for reaction and crystallization, controlling the pH value to be 6.2, and controlling the reaction time to be 40 minutes to obtain the high-quality calcium carbonate. And (3) carrying out solid-liquid separation on the slurry containing the calcium carbonate, and washing the filter cake to obtain calcium carbonate (2), wherein the filtrate is the filtrate containing magnesium chloride.

And introducing ammonia gas into the magnesium chloride filtrate, and controlling the pH value to be 8.0 to obtain magnesium hydroxide precipitate and an ammonium chloride solution. And (3) carrying out solid-liquid separation to obtain magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide.

And concentrating and crystallizing the separated ammonium chloride solution to obtain magnesium ammonium chloride crystals.

Calcium carbonate (1) obtained: purity: 58 percent;

calcium carbonate (2): purity: 97.2 percent;

magnesium hydroxide: purity: 97.1 percent;

ammonium chloride crystals: purity: 97.4 percent.

Implementation 4:

adding phosphate tailings (the main effective components of the phosphate tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state) and hydrochloric acid into a decomposition tank, and reacting for 45 minutes. And (3) carrying out solid-liquid separation on the reaction slurry, separating filtrate containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid which is an acid insoluble substance.

Adding ammonium bicarbonate into the filtrate containing calcium chloride and magnesium chloride, reacting and crystallizing, controlling the pH value to be 5.3, and controlling the reaction time to be 45 minutes to obtain the calcium carbonate containing impurities. And (3) carrying out solid-liquid separation on the slurry containing calcium carbonate, washing the filter cake with water to obtain calcium carbonate (1), continuously adding ammonium bicarbonate into the filtrate for reaction and crystallization, controlling the pH value to be 6.4, and controlling the reaction time to be 45 minutes to obtain the high-quality calcium carbonate. And (3) carrying out solid-liquid separation on the slurry containing the calcium carbonate, and washing the filter cake to obtain calcium carbonate (2), wherein the filtrate is the filtrate containing magnesium chloride.

And introducing ammonia gas into the magnesium chloride filtrate, and controlling the pH value to be 8.5 to obtain magnesium hydroxide precipitate and an ammonium chloride solution. And (3) carrying out solid-liquid separation to obtain magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide.

And concentrating and crystallizing the separated ammonium chloride solution to obtain magnesium ammonium chloride crystals.

Calcium carbonate (1) obtained: purity: 58 percent;

calcium carbonate (2): purity: 97.5 percent;

magnesium hydroxide: purity: 97.3 percent;

ammonium chloride crystals: purity: 97 percent.

Implementation 5:

adding phosphate tailings (the main effective components of the phosphate tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state) and hydrochloric acid into a decomposition tank, reacting for 30 minutes, carrying out solid-liquid separation on reaction slurry, separating filtrate containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid acid-insoluble substances.

Adding ammonium bicarbonate into filtrate containing calcium chloride and magnesium chloride, reacting and crystallizing, controlling the pH value to be 4.8, controlling the reaction time to be 30 minutes to obtain calcium carbonate containing impurities, carrying out solid-liquid separation on slurry containing the calcium carbonate, washing a filter cake to obtain calcium carbonate (1), feeding a solution containing the calcium carbonate into a cyclone, rotating at the speed of more than 7 m/min for 5-10 minutes, discharging the solution out of the cyclone, mixing with the ammonium bicarbonate, reacting and crystallizing, controlling the pH value to be 5.8, and controlling the reaction time to be 30 minutes to obtain the high-quality calcium carbonate. Carrying out solid-liquid separation on the slurry containing calcium carbonate, and washing a filter cake to obtain calcium carbonate (2), wherein the filtrate is a filtrate containing magnesium chloride;

and introducing ammonia gas into the magnesium chloride filtrate, and controlling the pH value to be 8 to obtain magnesium hydroxide precipitate and an ammonium chloride solution. And (3) carrying out solid-liquid separation to obtain magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide.

And concentrating and crystallizing the separated ammonium chloride solution to obtain magnesium ammonium chloride crystals.

Calcium carbonate (1) obtained: purity: 50 percent;

calcium carbonate (2): purity: 98.5 percent;

magnesium hydroxide: purity: 98.3 percent;

ammonium chloride crystals: purity: 97.1 percent.

Implementation 6:

adding the phosphate tailings (the main effective components of the phosphate tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state) and hydrochloric acid into a decomposition tank, reacting for 40 minutes, carrying out solid-liquid separation on reaction slurry, separating filtrate containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid acid-insoluble substances.

Adding ammonium bicarbonate into filtrate containing calcium chloride and magnesium chloride, reacting and crystallizing, controlling the pH value to be 5, controlling the reaction time to be 40 minutes to obtain calcium carbonate containing impurities, carrying out solid-liquid separation on slurry containing the calcium carbonate, washing a filter cake to obtain calcium carbonate (1), feeding a solution containing the calcium carbonate into a cyclone, rotating at a speed of more than 7 m/min for 5-10 minutes, discharging the solution out of the cyclone, mixing with the ammonium bicarbonate, reacting and crystallizing, controlling the pH value to be 6, and controlling the reaction time to be 40 minutes to obtain high-quality calcium carbonate. Carrying out solid-liquid separation on the slurry containing calcium carbonate, and washing a filter cake to obtain calcium carbonate (2), wherein the filtrate is a filtrate containing magnesium chloride;

and introducing ammonia gas into the magnesium chloride filtrate, and controlling the pH value to be 8 to obtain magnesium hydroxide precipitate and an ammonium chloride solution. And (3) carrying out solid-liquid separation to obtain magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide.

And concentrating and crystallizing the separated ammonium chloride solution to obtain magnesium ammonium chloride crystals.

Calcium carbonate (1) obtained: purity: 58 percent;

calcium carbonate (2): purity: 98.5 percent;

magnesium hydroxide: purity: 98.4 percent;

ammonium chloride crystals: purity: 98.1 percent.

Implementation 7:

adding phosphate tailings (the main effective components of the phosphate tailings comprise 1-8% by mass, 20-40% by mass and 5-20% by mass in terms of oxidation state) and hydrochloric acid into a decomposition tank, reacting for 45 minutes, carrying out solid-liquid separation on reaction slurry, separating filtrate containing calcium chloride and magnesium chloride, and washing a filter cake to obtain solid acid-insoluble substances.

Adding ammonium bicarbonate into filtrate containing calcium chloride and magnesium chloride, reacting and crystallizing, controlling the pH value to be 5, controlling the reaction time to be 40 minutes to obtain calcium carbonate containing impurities, carrying out solid-liquid separation on slurry containing the calcium carbonate, washing a filter cake to obtain calcium carbonate (1), feeding a solution containing the calcium carbonate into a cyclone, rotating at a speed of more than 7 m/min for 5-10 minutes, discharging the solution out of the cyclone, mixing with the ammonium bicarbonate, reacting and crystallizing, controlling the pH value to be 6.2, and controlling the reaction time to be 40 minutes to obtain high-quality calcium carbonate. Carrying out solid-liquid separation on the slurry containing calcium carbonate, and washing a filter cake to obtain calcium carbonate (2), wherein the filtrate is a filtrate containing magnesium chloride;

and (3) cross-flow mixing the magnesium chloride-containing solution and liquid ammonia, and controlling the pH value to be 8.5 to obtain a magnesium hydroxide precipitate and an ammonium chloride solution. And (3) carrying out solid-liquid separation to obtain magnesium hydroxide solid, and washing the magnesium hydroxide solid to obtain high-quality magnesium hydroxide.

And concentrating and crystallizing the separated ammonium chloride solution to obtain magnesium ammonium chloride crystals.

Calcium carbonate (1) obtained: purity: 58 percent;

calcium carbonate (2): purity: 98.5 percent;

magnesium hydroxide: purity: 98.4 percent;

ammonium chloride crystals: purity: 99.3 percent.

Through the above comparative experiments, it was found that the addition of a rotator to rotationally accelerate the liquid in step 5 causes the calcium carbonate (2): the purity of the magnesium hydroxide and ammonium chloride crystals is obviously improved, the average influence on the purity is increased by more than 1 percent, and the purity of the ammonium chloride crystals is improved by 1 percent by mixing the magnesium chloride-containing solution and the liquid ammonia in a cross flow manner in the step 7.