阅读说明：本技术 一种含铁凹凸棒石的提纯和转白方法 (Method for purifying and whitening attapulgite containing iron ) 是由 张法智 徐杰 刘湉 雷晓东 孔祥贵 陈馨 于 2019-12-10 设计创作，主要内容包括：本发明提供了一种含铁凹凸棒石的提纯和转白方法,实现拓宽凹凸棒石的高值化应用前景。本发明利用六偏磷酸钠或焦磷酸钠除去含铁凹凸棒石原矿粉中的石英杂质,利用胶体磨使溶液充分混合,通过离心机使石英和与凹凸棒石分离,研磨烘干后,再利用盐酸或硫酸除去凹凸棒石中的铁和碳酸盐等杂质,最后得到颜色呈白色纯度较高的凹凸棒石。(The invention provides a method for purifying and whitening attapulgite containing iron, which realizes the widening of the high-valued application prospect of the attapulgite. According to the method, sodium hexametaphosphate or sodium pyrophosphate is used for removing quartz impurities in the iron-containing attapulgite raw ore powder, a colloid mill is used for fully mixing the solution, the quartz and the attapulgite are separated by a centrifugal machine, after grinding and drying, impurities such as iron, carbonate and the like in the attapulgite are removed by using hydrochloric acid or sulfuric acid, and finally the white attapulgite with high purity is obtained.)

1. A method for purifying and whitening attapulgite containing iron is characterized by comprising the following specific operation steps:

A. grinding the attapulgite raw ore containing iron by using a ball mill, and sieving to 120 meshes for later use; preparing 3-5 wt% of sodium hexametaphosphate or sodium pyrophosphate solution; adding the iron-containing attapulgite raw ore powder into a sodium hexametaphosphate or sodium pyrophosphate solution according to the water-soil mass ratio of 1:8-12, mixing in a colloid mill for 20-50min, and performing ultrasonic treatment for 3-8 min; firstly removing quartz impurities at the bottom by using low-speed centrifugation, then settling the suspended attapulgite containing iron by using high-speed centrifugation, drying the obtained attapulgite containing iron, and grinding;

B. preparing 1-5mol/L hydrochloric acid or sulfuric acid solution, adding the iron-containing attapulgite obtained in the step A into the hydrochloric acid or sulfuric acid solution according to the solid-liquid mass ratio of 1:6-10, heating and stirring on a magnetic stirrer until the solution is yellow and the attapulgite dispersed in the solution is white, stopping heating, separating the attapulgite and the yellow solution by high-speed centrifugation, finally washing with distilled water until the solution is neutral, drying, and grinding.

2. The method for purifying and whitening attapulgite containing iron according to claim 1, wherein the ultrasonic frequency is 40 khz.

3. The method for purifying and whitening attapulgite containing iron according to claim 1, wherein the speed of the low-speed centrifugation is 1500r/min and the speed of the high-speed centrifugation is 3000 r/min.

4. The method for purifying and whitening attapulgite containing iron according to claim 1, wherein the drying temperature is 70-100 ℃.

The technical field is as follows:

the invention belongs to the technical field of attapulgite purification, and particularly relates to a method for purifying and whitening attapulgite containing iron.

Background art:

the attapulgite serving as 'thousand-purpose soil' is widely applied to the fields of inorganic chemical industry, building material industry, agriculture, edible oil processing, medicines and the like due to good performances of adsorbability, rheological property, carrier property, catalytic property, plasticity, salt resistance, water absorption and the like, the storage capacity of the attapulgite in the county of Youzzi, Gansu province reaches 9.02 hundred million tons, accounts for 63 percent of the worldwide proven storage capacity, and is the first to live in the world stably. Attapulgite belongs to rare non-metal mineral species in the world. Our country is the world where attapulgite is mainly stored, and attapulgite in Gansu province is mainly distributed in Jingyuan county, Huining county and Linze county in Zhangye city. The attapulgite grade of the silver belongs to the medium upper part, according to the multipoint test result, the content is generally 25-50%, the highest ore point reaches 60%, and the development and utilization prospect is wide. The attapulgite has a unique crystal structure, is a natural one-dimensional nano material, is rich in various trace elements such as copper, zinc, vanadium, molybdenum, selenium, iodine, iron, boron and the like required by animal and plant organisms, can effectively fill up the deficiency of the trace elements in soil, and has wide application prospect in modern agriculture, particularly gobi agriculture.

However, the purity is not high, so that the attapulgite in Gansu province has few industrial chains at present, and except applying to attapulgite compound fertilizer and soil remediation, the attapulgite is mostly sold to other places at a low price. Compared with Xuyi attapulgite at Anhui China and China, the attapulgite at Gansu province has the advantages of abundant storage capacity, obvious defects, low quality of ore soil, wide application prospect of high-purity attapulgite, and capability of realizing high-value application of the attapulgite, so that the purification of the attapulgite at Gansu province is a problem urgently needed at present.

According to the research of attapulgite in Gansu province of China, and the like [ attapulgite in Gansu region mineral composition analysis [ J ] silicate report, 2013,32(11): 2362-; the attapulgite in the scramIk area has a quartz content slightly higher than that of Jing and all at 14-22%, wherein the quartz content of the ballast points of the scramIk bridge is the highest and reaches 21.8%; the content of feldspar in four typical mine points is over 12 percent, the content of feldspar in the Jingyuan area is slightly higher than that in the Linze area, and the content of the Jingyuan high bay mine points is up to 19.8 percent; jingyuan, Huining area attapulgite has dolomite content higher than that in the region of Lingzhou, and the content is 5-12%; the contents of chlorite, gypsum, montmorillonite, sepiolite, calcite and mica are not greatly different and are all lower than 7 percent; wherein the content of montmorillonite in red attapulgite is slightly higher than that of green attapulgite, and the content of montmorillonite in green attapulgite is slightly higher than that of red attapulgite. The silver city is a region with abundant reserves in Gansu province, but the purity is not high, and the attapulgite has high iron content and brick red color, so that the purification research is needed, and the basis is laid for high-value application of the attapulgite.

The invention content is as follows:

the invention aims to provide a method for purifying and whitening attapulgite containing iron, which realizes the widening of the high-valued application prospect of the attapulgite.

The method for purifying and whitening the attapulgite containing iron comprises the following steps:

A. grinding the attapulgite raw ore containing iron by using a ball mill, and sieving to 120 meshes for later use; preparing 3-5 wt% of sodium hexametaphosphate or sodium pyrophosphate solution; adding the iron-containing attapulgite raw ore powder into a sodium hexametaphosphate or sodium pyrophosphate solution according to the water-soil mass ratio of 1:8-12, mixing in a colloid mill for 20-50min, and performing ultrasonic treatment for 3-8 min; firstly removing quartz impurities at the bottom by using low-speed centrifugation, then settling the suspended attapulgite containing iron by using high-speed centrifugation, drying the obtained attapulgite containing iron, and grinding;

B. preparing 1-5mol/L hydrochloric acid or sulfuric acid solution, adding the iron-containing attapulgite obtained in the step A into the hydrochloric acid or sulfuric acid solution according to the solid-liquid mass ratio of 1:6-10, heating and stirring on a magnetic stirrer until the solution is yellow and the attapulgite dispersed in the solution is white, stopping heating, separating the attapulgite and the yellow solution by high-speed centrifugation, finally washing with distilled water until the solution is neutral, drying, and grinding.

The ultrasonic frequency is 40 khz.

The speed of the low-speed centrifugation is 1500r/min, and the speed of the high-speed centrifugation is 3000 r/min.

The drying temperature is 70-100 ℃.

According to the method, sodium hexametaphosphate or sodium pyrophosphate is used for removing quartz impurities in the iron-containing attapulgite raw ore powder, a colloid mill is used for fully mixing the solution, the quartz and the attapulgite are separated by a centrifugal machine, after grinding and drying, impurities such as iron, carbonate and the like in the attapulgite are removed by using hydrochloric acid or sulfuric acid, and finally the white attapulgite with high purity is obtained.

Drawings

FIG. 1 is a Scanning Electron Microscope (SEM) picture of iron-containing attapulgite produced by Gansu silver in examples 1-3. As can be seen, the attapulgite is rod-shaped, is attached to some impurities, has a width of only a few nanometers and a length of about hundreds of nanometers to a few micrometers.

FIG. 2 is a Scanning Electron Microscope (SEM) image of the purified attapulgite containing iron from Gansu silver in examples 1-3. As can be seen, the impurities are obviously reduced, and the rods are irregularly arranged.

FIG. 3 is a Transmission Electron Microscope (TEM) image of Attapulgite produced from Gansu silver in examples 1-3.

FIG. 4 is a Transmission Electron Microscope (TEM) image of the purified attapulgite containing iron from silver albo-marginata in example 1. As can be seen, there are only a few microscopic impurities and the rods are closely arranged.

FIG. 5 is the X-ray diffraction (XRD) pattern of the attapulgite containing iron produced by Gansu silver in example 1 after purification and before and after whitening. Before purification, a, and after purification, b shows that the crystal form of the attapulgite is more regular and the diffraction peak is enhanced after purification.

FIG. 6 is a comparison graph of the purified natural substance of the attapulgite raw ore soil containing iron from Gansu silver in example 1. The sodium hexametaphosphate is used for primary purification, and hydrochloric acid is used for whitening.

FIG. 7 is a comparison graph of the purified natural substance of the attapulgite raw ore soil containing iron from Gansu silver in example 2. The sodium pyrophosphate is used for primary purification, and hydrochloric acid is used for whitening.

FIG. 8 is a comparison graph of the purified natural substance of the attapulgite raw ore soil containing iron from Gansu silver in example 3. The sodium hexametaphosphate is used for primary purification, and sulfuric acid is used for whitening.

Detailed Description