阅读说明：本技术 一种制备无水氯化镁的方法和系统 (Method and system for preparing anhydrous magnesium chloride ) 是由 李生廷 张勇 马珍 董昌吉 祁小庆 王志军 马彦军 胡晓英 王金晶 莫延香 于 2021-08-02 设计创作，主要内容包括：本发明涉及制备无水氯化镁的方法和系统,其中方法包括,第一步骤,将氢氧化镁和氯化铵均匀混合,得到第一物料；第二步骤,将所述第一物料与氨气、氯化氢混合,冷却至150℃～200℃,得到第二物料；第三步骤,将所述第二物料在200℃～300℃,加热0.5至2h,得到第三物料；第四步骤,将所述第三物料在300℃～450℃,加热0.5至2h,得到第四物料；第五步骤,将所述第四物料在450℃～700℃,加热0.5至2h,得到无水氯化镁；其中,第三物料所在的气氛中,氯化氢气体的体积百分含量大于5％,氨气与氯化氢气体的摩尔比大于1。本发明在系统内部形成自循环,工艺简单,减少污染,无水氯化镁纯度提升。(The invention relates to a method and a system for preparing anhydrous magnesium chloride, wherein the method comprises a first step of uniformly mixing magnesium hydroxide and ammonium chloride to obtain a first material; a second step, mixing the first material with ammonia gas and hydrogen chloride, and cooling to 150-200 ℃ to obtain a second material; step three, heating the second material at 200-300 ℃ for 0.5-2 h to obtain a third material; step four, heating the third material at 300-450 ℃ for 0.5-2 h to obtain a fourth material; fifthly, heating the fourth material at 450-700 ℃ for 0.5-2 h to obtain anhydrous magnesium chloride; wherein, in the atmosphere of the third material, the volume percentage of the hydrogen chloride gas is more than 5 percent, and the molar ratio of the ammonia gas to the hydrogen chloride gas is more than 1. The invention forms self-circulation in the system, has simple process, reduces pollution and improves the purity of the anhydrous magnesium chloride.)

1. A method for preparing anhydrous magnesium chloride comprises the following steps,

a first step (S1) of uniformly mixing magnesium hydroxide and ammonium chloride to obtain a first material, wherein a molar ratio of the ammonium chloride to the magnesium hydroxide is 1.98 to 2.5;

a second step (S2) of mixing the first material with ammonia gas and hydrogen chloride, cooling to 150-200 ℃ to enable the ammonia gas and the hydrogen chloride to react to generate ammonium chloride, and co-condensing and mixing the ammonium chloride with the first material to obtain a second material;

a third step (S3) of heating the second material at 200-300 ℃ for 0.5-2 h to obtain a third material;

a fourth step (S4) of heating the third material at 300-450 ℃ for 0.5-2 h to obtain a fourth material;

a fifth step (S5) of heating the fourth material at 450-700 ℃ for 0.5-2 h to obtain anhydrous magnesium chloride;

wherein, in the second step (S2), the addition amounts of the ammonia gas and the hydrogen chloride are set as follows: the volume percentage of the hydrogen chloride gas in the atmosphere of the third material is more than 5 percent, and the molar ratio of the ammonia gas to the hydrogen chloride gas is more than 1.

2. The method according to claim 1, wherein, in the first step (S1), the molar ratio of ammonium chloride to magnesium hydroxide is 2.

3. The method according to claim 1, wherein in the second step (S2), the first material, ammonia gas, hydrogen chloride are co-condensed with a cooling tower (2): throwing the first material from the top end of the cooling tower (2), introducing the ammonia gas and the hydrogen chloride from the bottom of the cooling tower (2), and simultaneously introducing clean cold air from the bottom end of the cooling tower (2) to adjust the temperature in the cooling tower (2) to 150-180 ℃ to obtain a second material and cooling tail gas.

4. A method according to claim 3, wherein the cooled tail gas is discharged from the top of the cooling tower (2) and ammonium chloride and ammonia gas are recovered.

5. The process according to claim 1, wherein the third step (S3), the fourth step (S4) and the fifth step (S5) are carried out in the same reactor (3), the off-gas produced in the third step (S3), the fourth step (S4) and the fifth step (S5) being recycled to the second step (S2) to supplement ammonia and hydrogen chloride.

6. A system for preparing anhydrous magnesium chloride comprises,

the mixer (1) is used for uniformly mixing magnesium hydroxide and ammonium chloride to obtain a first material, wherein the molar ratio of the ammonium chloride to the magnesium hydroxide is 1.98-2.5;

the cooling tower (2) is used for mixing the first material with ammonia gas and hydrogen chloride, cooling to 150-200 ℃ to enable the ammonia gas and the hydrogen chloride to react to generate ammonium chloride, and co-condensing and mixing the ammonium chloride with the first material to obtain a second material;

the reactor (3) is used for heating the second material for 0.5 to 2 hours at the temperature of 200 to 300 ℃ to obtain a third material, heating the third material for 0.5 to 2 hours at the temperature of 300 to 450 ℃ to obtain a fourth material, and heating the fourth material for 0.5 to 2 hours at the temperature of 450 to 700 ℃ to obtain anhydrous magnesium chloride;

wherein, in the cooling tower (2), the adding amount of the added ammonia gas and the hydrogen chloride is set as follows: in the atmosphere of the third material in the reactor (3), the volume percentage of the hydrogen chloride gas is more than 5 percent, and the molar ratio of the ammonia gas to the hydrogen chloride gas is more than 1.

7. The system according to claim 6, wherein the reactor (3) has a feed end higher than a discharge end, and a first heating section, a second heating section and a third heating section are sequentially arranged from the feed end toward the discharge end, the first heating section pair having a temperature of 200 ℃ to 300 ℃, the second heating section having a temperature of 300 ℃ to 450 ℃, and the third heating section having a temperature of 450 ℃ to 700 ℃.

8. A system according to claim 6, wherein the off-gas outlet of the reactor (3) is arranged at the top of the feed end.

9. A system according to claim 6, wherein stirring means are provided in the cooling tower (2).

10. The system of claim 7, wherein the end of the first heating section and the end of the second heating section are respectively provided with an intermediate discharge port for discharging intermediate products.

Technical Field

The invention relates to the field of preparation of anhydrous magnesium chloride, in particular to a method and a system for preparing anhydrous magnesium chloride by using magnesium hydroxide.

Background

The prior production process for dehydrating magnesium chloride mainly comprises the following steps:

1. gas-shielded dehydration in anhydrous HCl or Cl₂The hydrated magnesium chloride is heated and dehydrated in the environment, and the generation of magnesium oxide is avoided. For example, the process for producing anhydrous magnesium chloride from a concentrated magnesium chloride solution developed by Norsk Hydro in Norway has the disadvantages of large amount of high-temperature HCl gas circulation, high energy consumption and serious equipment corrosion at high temperature.

2. The method comprises the steps of organic solvent distillation and molecular sieve dehydration, wherein the magnesium chloride hydrate is easily dissolved in a polar organic solvent, and the anhydrous alcohol solution of magnesium chloride can be obtained by distillation and molecular sieve adsorption. For example, Belchetz dissolves magnesium chloride hydrate with monohydric saturated fatty alcohol having a boiling point of 100 to 180 ℃, and evaporates water to obtain an anhydrous magnesium chloride solution. However, when the organic solvent is removed by further distillation, the organic reagent and magnesium chloride are decomposed, the anhydrous magnesium chloride product contains a large amount of carbon and magnesium oxide and cannot be used as an electrolysis raw material, and the obtained anhydrous magnesium chloride solution needs to be further separated to prepare anhydrous magnesium chloride.

3. Decomposition dehydration method of complex of magnesium chloride double salt and potassiumCarnallite, ammonium carnallite and magnesium chloride hexammoniate are intermediates for preparing anhydrous magnesium chloride by decomposition, potassium carnallite is easy to dehydrate, and the decomposition rate of magnesium chloride in the dehydration process is low. The good reference of Yang nations refers to the technology of former Soviet Union, and carnallite is used as raw material for smelting magnesium after boiling, dewatering and melt chlorination. Research on the decomposition process of ammonium carnallite by Dolezal et al found that sublimation and decomposition of ammonium chloride produced HCl and NH₃And the like, so that the complex salt is prepared by using hydrochloride of amines (such as ethylenediamine, triethylamine and aniline) and hydrated magnesium chloride or brine instead, and the anhydrous magnesium chloride is prepared by decomposition, and the preparation process is complex and is easy to cause pollution.

In view of the above problems in the existing methods for preparing anhydrous magnesium chloride, how to reduce the requirements of the anhydrous magnesium chloride on reagents, reduce pollution and simplify the process becomes a problem to be solved urgently.

Disclosure of Invention

In order to solve the above problems, the present invention provides a method for preparing anhydrous magnesium chloride, comprising, as a first step S1, uniformly mixing magnesium hydroxide and ammonium chloride to obtain a first material, wherein the molar ratio of ammonium chloride to magnesium hydroxide is 1.98 to 2.5; a second step S2, mixing the first material with ammonia gas and hydrogen chloride, cooling to 150-200 ℃ to enable the ammonia gas and the hydrogen chloride to react to generate ammonium chloride, and co-condensing and mixing the ammonium chloride with the first material to obtain a second material; step S3, heating the second material at 200-300 ℃ for 0.5-2 h to obtain a third material; a fourth step S4, heating the third material at 300-450 ℃ for 0.5-2 h to obtain a fourth material; a fifth step S5, heating the fourth material at 450-700 ℃ for 0.5-2 h to obtain anhydrous magnesium chloride; in the second step S2, the addition amounts of the ammonia gas and the hydrogen chloride are set as follows: the volume percentage of the hydrogen chloride gas in the atmosphere of the third material is more than 5 percent, and the molar ratio of the ammonia gas to the hydrogen chloride gas is more than 1.

According to an embodiment of the present invention, in the first step S1, the molar ratio of ammonium chloride to magnesium hydroxide is 2.

According to an embodiment of the present invention, in the second step S2, the first material, ammonia gas, and hydrogen chloride are co-condensed by using the cooling tower 2: throwing the first material from the top end of the cooling tower 2, introducing the ammonia gas and the hydrogen chloride from the bottom of the cooling tower 2, and simultaneously introducing clean cold air from the bottom end of the cooling tower 2 to adjust the temperature in the cooling tower 2 to 150-180 ℃ to obtain a second material and cooling tail gas.

According to one embodiment of the invention, the cooled tail gas is discharged from the top of the cooling tower 2, and ammonium chloride and ammonia gas are recovered.

According to one embodiment of the invention, the third step S3, the fourth step S4 and the fifth step S5 are carried out in the same reactor 3, and the off-gas produced in the third step S3, the fourth step S4 and the fifth step S5 is recycled to the second step S2 to supplement ammonia gas and hydrogen chloride.

According to another aspect of the present invention, there is provided a system for preparing anhydrous magnesium chloride, comprising a mixer 1 for uniformly mixing magnesium hydroxide and ammonium chloride to obtain a first material, wherein the molar ratio of ammonium chloride to magnesium hydroxide is 1.98 to 2.5; the cooling tower 2 is used for mixing the first material with ammonia gas and hydrogen chloride, cooling to 150-200 ℃ to enable the ammonia gas and the hydrogen chloride to react to generate ammonium chloride, and co-condensing and mixing the ammonium chloride with the first material to obtain a second material; the reactor 3 is used for heating the second material for 0.5 to 2 hours at the temperature of 200 to 300 ℃ to obtain a third material, heating the third material for 0.5 to 2 hours at the temperature of 300 to 450 ℃ to obtain a fourth material, and heating the fourth material for 0.5 to 2 hours at the temperature of 450 to 700 ℃ to obtain anhydrous magnesium chloride; wherein, in the cooling tower 2, the adding amount of the added ammonia gas and the hydrogen chloride is set as follows: in the atmosphere of the third material in the reactor 3, the volume percentage of the hydrogen chloride gas is more than 5%, and the molar ratio of the ammonia gas to the hydrogen chloride gas is more than 1.

According to one embodiment of the present invention, the feeding end of the reactor 3 is higher than the discharging end, and a first heating section, a second heating section and a third heating section are sequentially arranged along the direction from the feeding end to the discharging end, wherein the temperature of the first heating section pair is 200 ℃ to 300 ℃, the temperature of the second heating section pair is 300 ℃ to 450 ℃, and the temperature of the third heating section pair is 450 ℃ to 700 ℃.

According to one embodiment of the invention, the off-gas outlet of the reactor 3 is arranged at the top of the feed end.

According to one embodiment of the invention, a stirring device is provided in the cooling tower 2.

According to one embodiment of the invention, the end of the first heating section and the end of the second heating section are respectively provided with an intermediate discharging hole for discharging intermediate products.

According to the invention, firstly, ammonium chloride and magnesium hydroxide solid particles are mixed, then ammonium chloride generated by the reaction of gaseous ammonia gas and hydrogen chloride is coated on the surface of magnesium hydroxide in a condensation mode, and finally, moisture is removed by a three-stage heating and removing method under the condition of ammonia gas and hydrogen chloride atmosphere to obtain anhydrous magnesium chloride. The solid-phase reaction of magnesium hydroxide and ammonium chloride is fully carried out by controlling the adding amount of the ammonium chloride; adding ammonia gas and hydrogen chloride to make the atmosphere contain more than 5% of hydrogen chloride and be alkalescent; the ammonium chloride and the magnesium hydroxide are fully contacted in a co-condensation mode, so that the solid-phase reaction is promoted; the tail gas formed in the three-section heating step can be directly utilized to the co-condensation step, self-circulation is formed in the system, and the emission is reduced, so that the pollution is reduced.

Drawings

FIG. 1 is a schematic representation of the steps of a process for preparing anhydrous magnesium chloride;

FIG. 2 is a schematic diagram of a system for preparing anhydrous magnesium chloride.

Detailed Description

In the following detailed description of the preferred embodiments of the invention, reference is made to the accompanying drawings that form a part hereof, and in which is shown by way of illustration, specific features of the invention, such that the advantages and features of the invention may be more readily understood and appreciated. The following description is an embodiment of the claimed invention, and other embodiments related to the claims not specifically described also fall within the scope of the claims.

Figure 1 shows a schematic step diagram of a process for preparing anhydrous magnesium chloride.

As shown in fig. 1, a method for preparing anhydrous magnesium chloride includes, as a first step S1, uniformly mixing magnesium hydroxide and ammonium chloride to obtain a first material, wherein the molar ratio of ammonium chloride to magnesium hydroxide is 1.98 to 2.5; a second step S2, mixing the first material with ammonia gas and hydrogen chloride, cooling to 150-200 ℃ to enable the ammonia gas and the hydrogen chloride to react to generate ammonium chloride, and co-condensing and mixing the ammonium chloride with the first material to obtain a second material; step S3, heating the second material at 200-300 ℃ for 0.5-2 h to obtain a third material; a fourth step S4, heating the third material at 300-450 ℃ for 0.5-2 h to obtain a fourth material; a fifth step S5, heating the fourth material at 450-700 ℃ for 0.5-2 h to obtain anhydrous magnesium chloride; in the second step S2, the addition amounts of the ammonia gas and the hydrogen chloride are set as follows: the volume percentage of the hydrogen chloride gas in the atmosphere of the third material is more than 5 percent, and the molar ratio of the ammonia gas to the hydrogen chloride gas is more than 1.

The method for preparing the anhydrous magnesium chloride adopts the magnesium hydroxide which is low in price and easy to obtain as a raw material, and adopts the principle that the sewage magnesium chloride with higher purity is obtained by utilizing the reaction of ammonium chloride and the magnesium hydroxide and providing a gas atmosphere at the same time and heating to remove water vapor, ammonia gas and hydrogen chloride gas.

In the first step S1, the magnesium hydroxide and the ammonium chloride are both solid particles or powder, and the magnesium hydroxide and the ammonium chloride can be uniformly mixed by a stirring device, and the magnesium hydroxide and the ammonium chloride are uniformly mixed in the physical sense all the time at normal temperature, that is, the first material is a uniform mixture of ammonium chloride particles and magnesium hydroxide particles.

The molar ratio of ammonium chloride to magnesium hydroxide is 1.98 to 2.5 and is mixed so that the magnesium to chlorine ratio is at least 1:2, i.e. ideally the magnesium to chlorine ratio is 1:2, more preferably the chlorine is in excess of 1: 2.02, so that the magnesium hydroxide can be reacted sufficiently. In the present invention, for the sake of distinction, this part of ammonium chloride is referred to as first ammonium chloride, and ammonium chloride generated by the reaction of ammonia gas and hydrogen chloride in the second step S2 is referred to as second ammonium chloride. The amount of the first ammonium chloride is calculated as the amount used for the reaction with magnesium hydroxide to form magnesium chloride, during which the magnesium chloride is reacted with magnesium hydroxide upon heating above 200 c in the third step S3, i.e. starting from 200 c, the magnesium hydroxide undergoes a solid phase reaction with ammonium chloride, releasing ammonia and water vapour.

When the first material is mixed with ammonia gas and hydrogen chloride gas and then is co-condensed, the ammonia gas and the hydrogen chloride gas react to generate ammonium chloride, namely second ammonium chloride, and the addition amount of the second ammonium chloride is mainly calculated according to the amount required for forming atmosphere.

Because the solid of the second ammonium chloride is generated under the condition that the ammonia gas and the hydrogen chloride gas are mixed with the first material and is condensed on the surface of the magnesium hydroxide particles in the first material or is doped into the first material, the solid of the second ammonium chloride and the first material are uniformly mixed or attached to the surface of the magnesium hydroxide particles, and therefore, the contact tightness between the ammonium chloride and the magnesium hydroxide is further enhanced, and the full reaction between the ammonium chloride and the magnesium hydroxide is facilitated.

In the second step S2, the generated water vapor and uncondensed gas are separated by cyclone and washed with water to recover ammonium chloride and ammonia, and the uncondensed gas mainly includes ammonia, hydrogen chloride, gaseous ammonium chloride, and the like.

In the present invention, the third step S3 to the fifth step S5 are three steps of heating and removing, which are generally performed in the same reactor 3, or may be performed in a plurality of reactors 3 connected in sequence, and in the third step S3, the temperature is controlled at 200 to 300 ℃, so that ammonium chloride and magnesium hydroxide react in a solid phase state, and a mixture of magnesium chloride hydrate and ammonium chloride is obtained, and the amount of the added ammonium chloride is controlled, so that the yield of the magnesium chloride hydrate at this time should be 90% or more. The third material is mainly magnesium chloride hydrate, and a small amount of magnesium hydroxide and ammonium chloride. When the temperature rises to the fourth step S4, the temperature rises to 300-450 ℃, the ammonium chloride in the third material almost completely reacts, a part of the ammonium chloride continues to react with the remaining small amount of magnesium hydroxide, most of the ammonium chloride is decomposed into ammonia gas and hydrogen chloride, an atmosphere of hydrogen chloride and ammonia gas is formed in the reactor 3, and at the moment, under the protection of the atmosphere, the magnesium chloride hydrate starts to remove crystal water, that is, the fourth material is mainly magnesium chloride hydrate. When the fifth step S5 is carried out, the temperature is continuously raised to be in the range of 450-700 ℃, and the crystal water in the magnesium chloride hydrate is finally removed, thereby obtaining the anhydrous magnesium chloride.

In the second step S2, the amounts of ammonia and hydrogen chloride added are controlled to be: the volume percentage of the hydrogen chloride gas in the atmosphere of the third material is more than 5 percent, so that basic magnesium chloride is prevented from being hydrolyzed in the removing process, and the purity of the anhydrous magnesium chloride is improved; the molar ratio of the ammonia gas to the hydrogen chloride gas is more than 1, so that the ammonia gas and the hydrogen chloride gas are alkalescent in the reactor 3, the corrosion to equipment is reduced, and meanwhile, the tail gas in the reactor 3 is used for supplementing the ammonia gas and the hydrogen chloride in the second step S2 to form the cyclic utilization in the system.

According to the invention, firstly, ammonium chloride and magnesium hydroxide solid particles are mixed, then ammonium chloride generated by the reaction of gaseous ammonia gas and hydrogen chloride is coated on the surface of magnesium hydroxide in a condensation mode, and finally, moisture is removed by a three-stage heating and removing method under the condition of ammonia gas and hydrogen chloride atmosphere to obtain anhydrous magnesium chloride. The solid-phase reaction of magnesium hydroxide and ammonium chloride is fully carried out by controlling the adding amount of the ammonium chloride; adding ammonia gas and hydrogen chloride to make the atmosphere contain more than 5% of hydrogen chloride and be alkalescent; the ammonium chloride and the magnesium hydroxide are fully contacted in a co-condensation mode, so that the solid-phase reaction is promoted; the tail gas formed in the three-section heating step can be directly utilized to the co-condensation step, self-circulation is formed in the system, and the emission is reduced, so that the pollution is reduced.

According to an embodiment of the present invention, in the first step S1, the molar ratio of ammonium chloride to magnesium hydroxide is 2.

According to an embodiment of the present invention, in the second step S2, the first material, ammonia gas, and hydrogen chloride are co-condensed by using the cooling tower 2: throwing the first material from the top end of the cooling tower 2, introducing the ammonia gas and the hydrogen chloride from the bottom of the cooling tower 2, and simultaneously introducing clean cold air from the bottom end of the cooling tower 2 to adjust the temperature in the cooling tower 2 to 150-180 ℃ to obtain a second material and cooling tail gas.

The cooling tower 2 may adopt any cooling tower 2 existing or invented in the future, and the invention is not limited. The first material is scattered from the top of the cooling tower 2, falls towards the bottom of the cooling tower 2, and simultaneously ammonia gas and hydrogen chloride are introduced from the bottom of the cooling tower, and when the first material falls, the traveling direction of the first material is opposite to that of the ammonia gas and the hydrogen chloride, and convection is formed. The ammonia gas and the hydrogen chloride react to form ammonium chloride solid, and the ammonium chloride solid is formed on the surface of the first material or independently formed into particles and falls down to the bottom of the cooling tower 2 together with the first material.

The first material is thrown the in-process of whereabouts, condenses the ammonium chloride to first material particle surface or mixes with first material particle, can make first material closely surround by the ammonium chloride, and the follow-up ammonia and the hydrogen chloride atmosphere of formation of being convenient for to and make the contact reaction probability increase of hydrogen chloride and magnesium hydroxide, the speed that takes place solid phase reaction accelerates, and the reaction degree is thorough.

According to one embodiment of the invention, the cooled tail gas is discharged from the top of the cooling tower 2, and ammonium chloride and ammonia gas are recovered. The ammonia gas and the ammonium chloride are recovered, and the hydrogen chloride is absorbed by water, so that the environmental pollution is avoided.

According to one embodiment of the present invention, in the method, the third step S3, the fourth step S4 and the fifth step S5 are performed in the same reactor 3, and the off-gas generated in the third step S3, the fourth step S4 and the fifth step S5 is recycled to the second step S2 to supplement ammonia gas and hydrogen chloride.

Figure 2 shows a schematic diagram of a system for preparing anhydrous magnesium chloride.

As shown in fig. 2, a system for preparing anhydrous magnesium chloride comprises a mixer 1 for uniformly mixing magnesium hydroxide and ammonium chloride to obtain a first material, wherein the molar ratio of the ammonium chloride to the magnesium hydroxide is 1.98-2.5; the cooling tower 2 is used for mixing the first material with ammonia gas and hydrogen chloride, cooling to 150-200 ℃ to enable the ammonia gas and the hydrogen chloride to react to generate ammonium chloride, and co-condensing and mixing the ammonium chloride with the first material to obtain a second material; the reactor 3 is used for heating the second material for 0.5 to 2 hours at the temperature of 200 to 300 ℃ to obtain a third material, heating the third material for 0.5 to 2 hours at the temperature of 300 to 450 ℃ to obtain a fourth material, and heating the fourth material for 0.5 to 2 hours at the temperature of 450 to 700 ℃ to obtain anhydrous magnesium chloride; wherein, in the cooling tower 2, the adding amount of the added ammonia gas and the added hydrogen chloride is set as follows: in the atmosphere of the third material in the reactor 3, the volume percentage of the hydrogen chloride gas is more than 5%, and the molar ratio of the ammonia gas to the hydrogen chloride gas is more than 1.

The mixer 1 is a stirring device, and in the invention, the mixer 1, the cooling tower 2 and the reactor 3 are arranged in a closed manner, namely, the contact with external moisture is reduced.

The mixer 1 is used for stirring and mixing ammonium chloride particles and magnesium hydroxide particles uniformly, then conveying the mixture into the cooling tower 2, scattering the mixture from the top of the cooling tower 2, mixing the mixture with hydrogen chloride and ammonia gas input from the bottom of the cooling tower 2 while falling, cooling the mixture to 150-200 ℃, synthesizing ammonium chloride, condensing the ammonium chloride on the surface of the magnesium hydroxide particles or self-condensing the ammonium chloride into particles, mixing the particles with a first material, and falling to the bottom of the cooling tower 2 to obtain a second material. The cooling tower 2 conveys the second material to a material inlet of the reactor 3, the reactor 3 is divided into three sections, the temperature is sequentially from low to high, magnesium hydroxide and ammonium chloride generate solid-phase reaction at the temperature of more than 200 ℃, magnesium chloride hydrate is generated, the ammonium chloride is decomposed to form ammonia heat exchange hydrogen chloride atmosphere besides the reaction with the magnesium hydroxide, and the concentration of the ammonia heat exchange hydrogen chloride atmosphere is determined by the ammonium chloride condensed in the cooling tower 2 and the amount of the particles of the ammonium chloride added in the mixer 1. At the temperature of more than 300 ℃, the ammonium chloride is completely decomposed, the magnesium chloride hydrate begins to remove crystal water, and at the temperature of more than 450 ℃, the final removal of the crystal water is completed, and the obtained anhydrous magnesium chloride is relatively pure. The hydrogen chloride and ammonia in the tail gas can be conveyed to the cooling tower 2 again for co-condensation.

According to one embodiment of the present invention, the feeding end of the reactor 3 is higher than the discharging end, and a first heating section, a second heating section and a third heating section are sequentially arranged along the direction from the feeding end to the discharging end, wherein the temperature of the first heating section pair is 200 ℃ to 300 ℃, the temperature of the second heating section pair is 300 ℃ to 450 ℃, and the temperature of the third heating section pair is 450 ℃ to 700 ℃.

When reactor 3 is one, the feed end is higher than the discharge end, makes the second material from the feed end to the discharge end because of the dead weight whereabouts, can also make full use of the waste heat of tail gas preheats the material that gets into reactor 3.

The first heating section, the second heating section and the third heating section are sequentially connected, and large-scale continuous production can be carried out.

According to one embodiment of the invention, the off-gas outlet of the reactor 3 is arranged at the top of the feed end.

According to one embodiment of the invention, a stirring device is provided in the cooling tower 2. The second material is mixed uniformly.

According to one embodiment of the invention, the end of the first heating section and the end of the second heating section are respectively provided with an intermediate discharging hole for discharging intermediate products. The intermediate product produced by the sectional heating can be used for preparing a drying agent or a heating bag material.

According to the invention, firstly, ammonium chloride and magnesium hydroxide solid particles are mixed, then ammonium chloride generated by the reaction of gaseous ammonia gas and hydrogen chloride is coated on the surface of magnesium hydroxide in a condensation mode, and finally, moisture is removed by a three-stage heating and removing method under the condition of ammonia gas and hydrogen chloride atmosphere to obtain anhydrous magnesium chloride. The solid-phase reaction of magnesium hydroxide and ammonium chloride is fully carried out by controlling the adding amount of the ammonium chloride; adding ammonia gas and hydrogen chloride to make the atmosphere contain more than 5% of hydrogen chloride and be alkalescent; the ammonium chloride and the magnesium hydroxide are fully contacted in a co-condensation mode, so that the solid-phase reaction is promoted; tail gas formed in the three-section heating step can be directly utilized to the co-condensation step, self-circulation is formed in the system, and emission is reduced, so that pollution is reduced; the reactor sets up to the feed end and is higher than the discharge end, and the tail gas export sets up at the feed end, makes the material from feed end to discharge end because of the dead weight whereabouts, and the waste heat that can also make full use of tail gas preheats the material that gets into the reactor.

It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that those skilled in the art will be able to design alternative embodiments without departing from the scope of the appended claims. In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim.