阅读说明：本技术 一种生产高纯石英粉的耦合纯化工艺 (Coupling purification process for producing high-purity quartz powder ) 是由 陈海燕 于 2020-12-27 设计创作，主要内容包括：本发明提供一种生产高纯石英粉的耦合纯化工艺,包括如下步骤：1)粗选；2)浸泡；3)煅烧；4)水淬；5)球磨；6)磁选；7)焙烧；8)酸洗；9)浮选；10)水洗；11)烘干。所述纯化工艺将石英粉的生产与纯化流程进行耦合,在生产搞得过程中进行纯化,得到高纯度石英粉,生产工艺简单,生产成本低。(The invention provides a coupling purification process for producing high-purity quartz powder, which comprises the following steps: 1) roughing; 2) soaking; 3) calcining; 4) water quenching; 5) ball milling; 6) magnetic separation; 7) roasting; 8) acid washing; 9) flotation; 10) washing with water; 11) and (5) drying. The purification process couples the production of the quartz powder with the purification process, and the quartz powder is purified in the production obtaining process to obtain the high-purity quartz powder, and the purification process has the advantages of simple production process and low production cost.)

1. A coupling purification process for producing high-purity quartz powder is characterized by comprising the following steps:

1) roughing, removing floating soil and ash slag in the quartz ore;

2) soaking, namely soaking the roughly selected quartz ore in a primary pickling solution for 1-2 hours, wherein the primary pickling solution comprises the following components in parts by weight: hydrochloric acid: 20-30 parts of oxalic acid: 10-15 parts of deionized water: 50-60 parts;

3) calcining, namely feeding the soaked quartz ore into a calcining furnace for calcining, wherein the calcining temperature is 800-850 ℃, and the calcining time is 40-50 minutes;

4) water quenching, namely feeding the calcined quartz ore into cold water for rapid cooling, and drying after cooling;

5) ball milling, namely, finely crushing quartz ores, and then sending the quartz ores into a ball mill for ball milling to obtain quartz ore particles with the particle size of 150-180 meshes;

6) magnetic separation, namely selecting a permanent magnetic strong magnetic drum magnetic separator with the magnetic field intensity of 6000-8000 Gauss to carry out magnetic separation on the quartz ore particles obtained in the step 5);

7) roasting, namely roasting the quartz ore particles subjected to the magnetic separation treatment for 2-5 hours at the temperature of 300-1500 ℃;

8) acid washing, pouring the quartz ore particles treated in the step 7) into a mixed acid solution, stirring for 30-60 minutes at 50-60 ℃, filtering, washing filter residues with water until the pH value of the filtrate is 6-7 after water washing again, and collecting the filter residues;

9) and (3) flotation, namely adding the quartz ore particles subjected to acid washing into a flotation agent for flotation, wherein the flotation agent comprises the following components in parts by weight: kerosene: 50-60 parts of sodium carbonate: 15-25 parts of hexadecyl dimethyl benzyl ammonium chloride: 5-10 parts of nonylphenol polyoxyethylene ether: 10-15 parts of ethylene glycol ethyl ether: 5-10 parts of ethanol: 5-10 parts of a coupling agent: 1-5 parts of a surfactant: 1-5 parts;

10) washing, namely washing the filter residue after the acid washing by using deionized water;

11) and drying to obtain the high-purity quartz powder.

2. The coupling purification process for producing high-purity quartz powder according to claim 1, characterized in that quartz ore with a silica grade of not less than 95% and an average diameter of 2-5 mm after crushing is selected in step 1).

3. The coupled purification process for producing high-purity quartz powder according to claim 1, wherein in the step 5), alumina balls or zirconia balls with the diameter of 25-35 mm are adopted for ball milling the quartz ore in a ball mill.

4. The coupled purification process for producing high-purity quartz powder according to claim 1, wherein the mixed acid solution used in step 8) comprises the following components in parts by weight: hydrochloric acid: 50-60 parts of phosphoric acid: 10-15 parts of N, N-dimethylformamide: 5-10 parts of persulfate: 5-10 parts of a surfactant: 1-5 parts of corrosion inhibitor: 1-5 parts of deionized water: 80-100 parts.

5. The coupled purification process for producing high-purity quartz powder as claimed in claim 4, wherein the surfactant in step 8) is fatty alcohol-polyoxyethylene ether.

6. The coupled purification process for producing high-purity quartz powder according to claim 4, wherein the corrosion inhibitor in step 8) is polyethylene glycol.

7. The coupled purification process for producing high-purity quartz powder according to claim 1, wherein the surfactant in step 9) is sodium dodecylbenzenesulfonate.

8. The coupled purification process for producing high purity quartz powder according to claim 1, wherein the coupling agent in step 9) is KH 550.

Technical Field

The invention belongs to the field of quartz powder production and purification, and particularly relates to a coupling purification process for producing high-purity quartz powder.

Background

The quartz powder (together with quartz sand) is also called silica micropowder. Quartz sand is a hard, wear-resistant, chemically stable silicate mineral, the main mineral component of which is SiO₂The quartz sand is milky white or colorless and semitransparent, has the hardness of 7, is crisp and has no cleavage, shell-shaped fracture, glossy grease, the density of 2.65 and the bulk density (20-200 meshes of 1.5), has obvious anisotropy in chemical, thermal and mechanical properties, is insoluble in acid, is slightly soluble in KOH solution and has the melting point of 1650 ℃.

The high-purity quartz powder is generally SiO₂The quartz micropowder with the content higher than 99.9 percent is mainly applied to the industries of IC integrated circuits, quartz glass and the like, and higher products thereof are more widely applied to large-scale and super-large-scale integrated circuits, optical fibers, lasers, aerospace and military. The high-purity quartz powder is a neutral inorganic filler, does not contain crystal water, does not participate in the chemical reaction of the filled material, is a very stable mineral filler, is widely applied to plastics, rubber, ceramics and coatings, and can increase the yieldThe product has various new functions, and can save a large amount of raw materials.

Most of the existing high-purity quartz powder is purified after the production of finished products, for example, chinese patent publication No. CN104556047B discloses a production process for preparing high-purity quartz powder from quartz rock, which comprises the following steps: 1) soaking; 2) crushing; 3) calcining; 4) water quenching; 5) grinding; 6) magnetic separation; 7) electrostatic separation; 8) acid washing; 9) washing with deionized water; 10) and (5) drying. However, the purification of the quartz powder requires separate treatment.

Disclosure of Invention

In order to solve the problems, the invention aims to provide a coupling purification process for producing high-purity quartz powder, which couples the production of the quartz powder with a purification process, and carries out purification in the production obtaining process to obtain the high-purity quartz powder, and the coupling purification process has the advantages of simple production process and low production cost.

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

a coupling purification process for producing high-purity quartz powder, which comprises the following steps:

1) roughing, removing floating soil and ash slag in the quartz ore;

2) soaking, namely soaking the roughly selected quartz ore in a primary pickling solution for 1-2 hours, wherein the primary pickling solution comprises the following components in parts by weight: hydrochloric acid: 20-30 parts of oxalic acid: 10-15 parts of deionized water: 50-60 parts;

3) calcining, namely feeding the soaked quartz ore into a calcining furnace for calcining, wherein the calcining temperature is 800-850 ℃, and the calcining time is 40-50 minutes;

4) water quenching, namely feeding the calcined quartz ore into cold water for rapid cooling, and drying after cooling;

5) ball milling, namely, finely crushing quartz ores, and then sending the quartz ores into a ball mill for ball milling to obtain quartz ore particles with the particle size of 150-180 meshes;

6) magnetic separation, namely selecting a permanent magnetic strong magnetic drum magnetic separator with the magnetic field intensity of 6000-8000 Gauss to carry out magnetic separation on the quartz ore particles obtained in the step 5);

7) roasting, namely roasting the quartz ore particles subjected to the magnetic separation treatment for 2-5 hours at the temperature of 300-1500 ℃;

8) acid washing, pouring the quartz ore particles treated in the step 7) into a mixed acid solution, stirring for 30-60 minutes at 50-60 ℃, filtering, washing filter residues with water until the pH value of the filtrate is 6-7 after water washing again, and collecting the filter residues;

9) and (3) flotation, namely adding the quartz ore particles subjected to acid washing into a flotation agent for flotation, wherein the flotation agent comprises the following components in parts by weight: kerosene: 50-60 parts of sodium carbonate: 15-25 parts of hexadecyl dimethyl benzyl ammonium chloride: 5-10 parts of nonylphenol polyoxyethylene ether: 10-15 parts of ethylene glycol ethyl ether: 5-10 parts of ethanol: 5-10 parts of a coupling agent: 1-5 parts of a surfactant: 1-5 parts;

10) washing, namely washing the filter residue after the acid washing by using deionized water;

11) and drying to obtain the high-purity quartz powder.

Further, in the step 1), quartz ore with the grade of silicon dioxide being more than or equal to 95% and the average diameter being 2-5 mm after being crushed is selected.

Further, in the step 5), alumina balls or zirconia balls with the diameter of 25-35 mm are adopted to ball-mill the quartz ore in a ball mill.

Further, the mixed acid solution used in the step 8) comprises the following components in parts by weight: hydrochloric acid: 50-60 parts of phosphoric acid: 10-15 parts of N, N-dimethylformamide: 5-10 parts of persulfate: 5-10 parts of a surfactant: 1-5 parts of corrosion inhibitor: 1-5 parts of deionized water: 80-100 parts.

Further, in the step 8), the surfactant is fatty alcohol-polyoxyethylene ether.

Further, in the step 8), the corrosion inhibitor is polyethylene glycol.

Further, the surfactant in the step 9) is sodium dodecyl benzene sulfonate.

Further, the coupling agent in step 9) is KH 550.

The invention has the beneficial effects that:

the purification process couples the production and purification processes of the quartz powder, the quartz powder is purified in the production process, a specially-made primary pickling solution is used for soaking and pickling, a specially-made mixed acid solution is used for carrying out secondary pickling to form twice pickling, and a specially-made flotation agent is used for carrying out flotation, so that the high-purity quartz powder is obtained, and the purification process is simple and low in production cost.

Detailed Description

The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.

Example 1

The invention relates to a coupling purification process for producing high-purity quartz powder, which comprises the following steps:

1) roughing, removing floating soil and ash slag in the quartz ore;

2) soaking, namely soaking the roughly selected quartz ore in a primary pickling solution for 1-2 hours, wherein the primary pickling solution comprises the following components in parts by weight: hydrochloric acid: 20-30 parts of oxalic acid: 10-15 parts of deionized water: 50-60 parts;

3) calcining, namely feeding the soaked quartz ore into a calcining furnace for calcining, wherein the calcining temperature is 800-850 ℃, and the calcining time is 40-50 minutes;

4) water quenching, namely feeding the calcined quartz ore into cold water for rapid cooling, and drying after cooling;

5) ball milling, namely, finely crushing quartz ores, and then sending the quartz ores into a ball mill for ball milling to obtain quartz ore particles with the particle size of 150-180 meshes;

6) magnetic separation, namely selecting a permanent magnetic strong magnetic drum magnetic separator with the magnetic field intensity of 6000-8000 Gauss to carry out magnetic separation on the quartz ore particles obtained in the step 5);

7) roasting, namely roasting the quartz ore particles subjected to the magnetic separation treatment for 2-5 hours at the temperature of 300-1500 ℃;

8) acid washing, pouring the quartz ore particles treated in the step 7) into a mixed acid solution, stirring for 30-60 minutes at 50-60 ℃, filtering, washing filter residues with water until the pH value of the filtrate is 6-7 after water washing again, and collecting the filter residues;

9) and (3) flotation, namely adding the quartz ore particles subjected to acid washing into a flotation agent for flotation, wherein the flotation agent comprises the following components in parts by weight: kerosene: 50-60 parts of sodium carbonate: 15-25 parts of hexadecyl dimethyl benzyl ammonium chloride: 5-10 parts of nonylphenol polyoxyethylene ether: 10-15 parts of ethylene glycol ethyl ether: 5-10 parts of ethanol: 5-10 parts of a coupling agent: 1-5 parts of a surfactant: 1-5 parts;

10) washing, namely washing the filter residue after the acid washing by using deionized water;

11) and drying to obtain the high-purity quartz powder.

Further, in the step 1), quartz ore with the grade of silicon dioxide being more than or equal to 95% and the average diameter being 2-5 mm after being crushed is selected.

Further, in the step 5), alumina balls or zirconia balls with the diameter of 25-35 mm are adopted to ball-mill the quartz ore in a ball mill.

Further, the mixed acid solution used in the step 8) comprises the following components in parts by weight: hydrochloric acid: 50-60 parts of phosphoric acid: 10-15 parts of N, N-dimethylformamide: 5-10 parts of persulfate: 5-10 parts of a surfactant: 1-5 parts of corrosion inhibitor: 1-5 parts of deionized water: 80-100 parts.

Further, in the step 8), the surfactant is fatty alcohol-polyoxyethylene ether.

Further, in the step 8), the corrosion inhibitor is polyethylene glycol.

Further, the surfactant in the step 9) is sodium dodecyl benzene sulfonate.

Further, the coupling agent in step 9) is KH 550.

The coupling purification process for producing high-purity quartz powder disclosed by the invention couples the production and purification processes of the quartz powder, carries out purification in the production process, adopts specially-made primary pickling liquid for soaking and pickling, adopts specially-made mixed acid solution for carrying out secondary pickling to form twice pickling, and adopts a specially-made flotation agent for carrying out flotation, so that the high-purity quartz powder is obtained, and the coupling purification process is simple in production process and low in production cost.

It should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the present invention.