阅读说明：本技术 一种微米级超细氯化钠的制备方法 (Preparation method of micron-sized superfine sodium chloride ) 是由 邓强 邱常义 胡景 孙七林 李春林 宋信信 熊泽华 于 2019-11-05 设计创作，主要内容包括：本发明提供一种微米级超细氯化钠的制备方法,即采用溶解度差异制备微米级超细化钠的方法。氯化钠溶于水或用液体盐制成饱和氯化钠溶液,然后加入溶解度比氯化钠大的无机盐,并添加抗凝结剂,搅拌,快速过滤收集结晶,固体再用饱和氯化钠溶液洗涤,固体再于真空干燥箱中80℃干燥制得微米级超细氯化钠粉体。若为含钙无机盐制备的滤液可再加入芒硝搅拌,再过滤,固体再用水洗涤,制备超细硫酸钙,滤液再用于制备液体盐。若为含铵无机盐制备的滤液,可作为液体肥使用。本发明工艺简单,原材料简单,成本较低,无废水排放。(The invention provides a preparation method of micron-sized superfine sodium chloride, namely a method for preparing micron-sized superfine sodium by adopting solubility difference. Dissolving sodium chloride in water or preparing saturated sodium chloride solution with liquid salt, adding inorganic salt with solubility greater than that of sodium chloride, adding anti-coagulating agent, stirring, filtering quickly to collect crystal, washing the solid with saturated sodium chloride solution, and drying the solid in vacuum drying oven at 80 deg.C to obtain micron-level superfine sodium chloride powder. If the filtrate is prepared from calcium-containing inorganic salt, adding Natrii sulfas, stirring, filtering, washing the solid with water, preparing superfine calcium sulfate, and using the filtrate to prepare liquid salt. If the filtrate is prepared from inorganic salt containing ammonium, the filtrate can be used as liquid fertilizer. The invention has simple process, simple raw materials, lower cost and no wastewater discharge.)

1. A preparation method of micron-sized superfine sodium chloride is characterized by comprising the following specific steps:

a. adding inorganic salt into saturated sodium chloride solution, stirring, precipitating sodium chloride, adding an anti-coagulating agent, quickly filtering, and collecting crystals and filtrate;

b. washing the precipitated sodium chloride crystal with saturated sodium chloride solution for 3-5 times, and vacuum drying at 80 deg.C to obtain micron-sized superfine sodium chloride.

2. The method for preparing micron-sized ultrafine sodium chloride according to claim 1, wherein the saturated sodium chloride solution is any one of a saturated sodium chloride solution prepared by dissolving sodium chloride in water and a liquid salt at normal temperature, and the anti-agglomerating agent is potassium ferrocyanide.

3. The method for preparing micron-sized ultrafine sodium chloride according to claim 1, wherein the inorganic salt is an inorganic salt having a solubility greater than that of sodium chloride, and includes a calcium-containing inorganic salt and an ammonium-containing inorganic salt, and the inorganic salt is any one of an inorganic salt solid and an inorganic salt saturated solution.

4. The method for preparing micron-sized ultrafine sodium chloride according to claims 1 to 3, wherein the inorganic salt is an ammonium-containing inorganic salt, specifically any one of ammonium carbonate and ammonium formate.

5. The process according to claim 4, wherein the filtrate Cl is obtained in step a ^-The concentration is 3.55-3.65g/L, and the fertilizer is used as a liquid fertilizer.

6. The method for preparing micron-sized ultrafine sodium chloride according to any one of claims 1 to 3, wherein the inorganic salt is a calcium-containing inorganic salt _，In particular to any one of calcium chloride, calcium bromide, calcium iodide and calcium perchlorate.

7. The method according to claim 6, wherein the filtrate Ca in step a ²⁺The concentration is 200-220g/L, mirabilite is added and stirred to react until Ca is obtained ²⁺The concentration is 0.55-0.65g/L, filtering, washing the solid with water to prepare superfine calcium sulfate, and using the filtrate to prepare liquid salt.

8. The method according to claim 6, wherein the molar ratio of sulfate ions in said salt cake to calcium in said calcium-containing inorganic salt is 1: 1.

9. The method according to claim 6, wherein the inorganic salt is calcium chloride solid, and the amount of the calcium chloride solid is in a range of 100mL of a saturated sodium chloride solution to 74.2g of calcium chloride.

10. The method according to claim 6, wherein the inorganic salt is a saturated calcium chloride solution, and the volume ratio of the saturated calcium chloride solution to the saturated sodium chloride solution is 3: 1.

Technical Field

The invention relates to the field of domestic salt and medical salt, in particular to a preparation method of micron-sized superfine sodium chloride.

Background

The superfine sodium chloride is one of fine chemical products with high added value in salt products, and has the advantages of wide application, higher price and large market demand. The superfine sodium chloride can be roughly classified into the following three types according to the use and preparation method of the superfine powder: fine powder with particle size of 10-100 μm; micron-sized powder with the grain diameter of 1-10 mu m; submicron powder with the grain diameter of 0.1-1 μm.

The superfine sodium chloride is one of fine chemical products with high added value in salt products, and has wide application: (1) pore control agents in the preparation of porous materials (porous metals, porous ceramics, porous polymers); (2) the medical field. (3) The beauty industry and the like. (4) The superfine sodium chloride is an air disinfection material and is made into sodium chloride aerosol for air disinfection. (5) Metal fire extinguishing, sodium chloride powder extinguishing agent and other fields.

The preparation method of the superfine sodium chloride comprises a mechanical crushing method, a spray drying method, a liquid phase method, an anti-solvent method and a lamellar crystallization method. The mechanical crushing method has higher requirement on equipment, the obtained sodium chloride particles have irregular shapes, the purity of impurities is not high, the particle size distribution of processed powder particles is wider, the energy consumption is high, the sodium chloride is crushed to be less than 100 mu m, but the sodium chloride is difficult to break through to be less than 10 mu m and is impossible to reach the nanometer level; the spray drying method for preparing ultrafine crystals has the advantages of rapid drying process, direct powdering, high product purity, strong controllability and the like, but the requirement on the concentration of sodium chloride is high, the concentration can increase the viscosity of spray liquid, a nozzle is easy to block, the sprayed material can be agglomerated sometimes, the whole spray drying time can be prolonged if the concentration is too low, the energy consumption is increased, the prepared product is amorphous, the physical property is unstable, the recrystallization is easy to realize in a high-humidity environment, bridging is formed among particles, the particles are coarse, and only micron-sized sodium chloride can be prepared; although the liquid phase method, the anti-solvent method and the lamellar crystallization method which are researched in the prior art can be used for preparing the superfine sodium chloride, the yield is low, the particle size distribution range is extremely wide, the sodium chloride crystals with uniform particle size range, good dispersibility and complete crystallization cannot be prepared, an organic solvent is generally required, and the flammability and the flash point of the organic solvent are lower and have greater potential safety hazard due to the fact that the volatility of the organic solvent has higher requirements on pipelines and equipment. Foreign researchers have adopted an ultrasonic chemical method to prepare medical micron-sized superfine sodium chloride powder with the sodium chloride particle size of about 1200 meshes (about 10 microns), but the use of an ultrasonic technology has certain environmental hazards.

Disclosure of Invention

The invention aims to provide a preparation method of micron-sized superfine sodium chloride.

In order to achieve the purpose, the preparation method provided by the invention comprises the following specific steps:

a. adding inorganic salt into saturated sodium chloride solution, stirring, precipitating sodium chloride, adding an anti-coagulating agent, quickly filtering, and collecting crystals and filtrate;

b. washing the precipitated sodium chloride crystal with saturated sodium chloride solution for 3-5 times, and vacuum drying at 80-120 deg.C to obtain micron-sized superfine sodium chloride.

The saturated sodium chloride solution is any one of saturated sodium chloride solutions prepared by dissolving sodium chloride in water and liquid salt at normal temperature.

The inorganic salt is an inorganic salt with solubility greater than that of sodium chloride, and comprises a calcium-containing inorganic salt and an ammonium-containing inorganic salt.

The inorganic salt is any one of inorganic salt solid and saturated solution of the inorganic salt.

The anti-coagulating agent is potassium ferrocyanide.

Preferably, the first and second electrodes are formed of a metal,

the inorganic salt is an ammonium-containing inorganic salt, and specifically is any one of ammonium carbonate or ammonium formate.

Cl in the filtrate in the step a ^-The concentration is 3.55-3.65g/L, which indicates that the sodium chloride is basically completely precipitated.

The filtrate in the step a can be used as liquid fertilizer.

In particular to one of calcium chloride, ammonium carbonate, ammonium formate, calcium bromide, calcium iodide and calcium perchlorate.

Preferably, the first and second electrodes are formed of a metal,

the inorganic salt is calcium-containing inorganic salt, specifically any one of calcium chloride, calcium bromide, calcium iodide and calcium perchlorate.

Ca in the filtrate ²⁺The concentration was 200-220g/L, indicating complete precipitation of sodium chloride.

Adding mirabilite into the filtrate, stirring, and reacting to Ca ²⁺The concentration is 0.55-0.65g/L, filtering, washing the solid with water to prepare superfine calcium sulfate, and using the filtrate to prepare liquid salt;

the molar ratio of the mirabilite to the calcium in the calcium-containing inorganic salt is 1: 1.

Preferably, the first and second electrodes are formed of a metal,

the inorganic salt is calcium chloride solid;

the amount of calcium chloride solid was added as 100mL of saturated sodium chloride solution to 74.2g of calcium chloride.

Preferably, the first and second electrodes are formed of a metal,

the inorganic salt is a saturated calcium chloride solution;

the volume ratio of the saturated calcium chloride solution to the saturated sodium chloride solution is 3: 1.

The invention has the beneficial effects that:

the invention utilizes the solubility difference to prepare micron-sized superfine sodium, and adopts inorganic salt with the solubility higher than that of sodium chloride to dissolve in saturated sodium chloride solution to separate out the sodium chloride. When the inorganic salt is calcium salt, the filtrate for separating out sodium chloride can be added with mirabilite to prepare superfine calcium sulfate, and the filtrate can be used as a raw material for producing liquid salt. When the inorganic salt is ammonium salt, the filtrate separated out of the sodium chloride can be used as liquid fertilizer. Simple process, simple raw materials, low cost and no wastewater discharge.

The superfine sodium chloride prepared by the invention has the particle size of below 10 mu m, more regular shape, purity of above 99.5%, whiteness of above 95 and yield of about 70%.

Drawings

FIG. 1. sodium chloride of micron level in example 1

FIG. 2 micron-sized calcium sulfate of example 1

FIG. 3. sodium chloride of micron level in example 2

FIG. 4. sodium chloride of micron level in example 3

FIG. 5. sodium chloride of micron level in example 4

FIG. 6 micron-sized calcium sulfate of example 4

FIG. 7. sodium chloride of micron level in example 5

FIG. 8 micron-sized calcium sulfate of example 5

Detailed Description

In order to more clearly and completely describe the technical scheme of the invention, the invention is further described in detail by the specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the invention, and are not used for limiting the invention, and various changes can be made within the scope defined by the claims of the invention.