CN115069433A - Method and device for purifying attapulgite clay - Google Patents

Abstract

A method for purifying attapulgite clay of the present invention includes the following steps: Step A, crushing the attapulgite ore, adding water to the crushed attapulgite to prepare a suspension, adding it into a mixing bucket, and adjusting Slurry treatment to obtain attapulgite suspension; Step B, use the feeding pump to feed the attapulgite suspension obtained in Step A into the hydrocyclone, feed the materials evenly, and put the sorted hydrocyclone The underflow is collected, sorted again, and the overflow after the two separations is collected to obtain purified attapulgite clay. The present invention starts from the physical properties of attapulgite, attempts to dissociate attapulgite and gangue minerals by crushing and stirring and mixing, and uses a hydrocyclone for separation after sufficient dissociation. By adjusting the slurry concentration, feeding pressure, cone ratio of the cyclone and other conditions, it is separated to achieve the effect of purification.

Description

A kind of purification method and device of attapulgite clay

technical field

The invention relates to a method for hydraulic separation and purification of attapulgite clay, belonging to the field of attapulgite purification.

Background technique

Attapulgite, also known as Palygorskite, is a hydrous magnesium-rich silicate clay mineral with a chain-layered structure. Its structure is a 2:1 clay mineral, that is, two layers of silicon-oxygen tetrahedron and one layer of aluminum-oxygen octahedron. Due to its unique tetrahedral structure and a large number of nano-channels inside it, it has high utilization value. my country's attapulgite resources are mainly distributed in Jiangsu, Anhui, Gansu and other places. Although the resources are abundant, the grade of attapulgite ore is not high. With the development of the economy and the advancement of science and technology, the requirements for the purity of attapulgite are increasing day by day in all walks of life. Therefore, it is necessary to purify it.

At present, the purification method of attapulgite is mainly wet purification, which is purified by centrifugation after grinding, and is also synergistically treated by adding dispersant and ultrasonic treatment. Zheng Zhijie et al [Zheng Zhijie, Cheng Jigui, Xia Yonghong, et al. Research on the purification of attapulgite clay [J]. Bulletin of Silicate, 2013, 32(12): 2471-2475.] Direct centrifugation and centrifugal treatment after wet ball milling were used respectively. The attapulgite clay was purified by the method, and the purity of the attapulgite clay after purification could reach 82.4% and 95.3%, respectively. Chen Tianhu et al [Chen Tianhu, Peng Shuchuan, Huangchuan Hui, Shi Xiaoli, Feng Youliang. Preparation of pure attapulgite from Suwan attapulgite clay [J]. Journal of Silicate, 2004(08):965-969.] complexed with EDTA, treated with sodium carbonate and then The gangue minerals in the attapulgite are removed by centrifugation, and the purity of the purified sample is greater than 98%. Ren Jing et al. [Ren Jing, Zhao Tingting. Purification of attapulgite and characterization of its dispersion properties [J]. Modern State-owned Enterprise Research, 2015(20): 175-177] added dispersant sodium pyrophosphate to treat attapulgite, and passed Ultrasonic and centrifugal treatment were used to purify attapulgite. The results showed that the purity of the product reached approximately 100%, the specific surface area was increased, and the water absorption was enhanced. The shortcomings of the above methods are: high centrifugal force (2000-10000 r/min) is required, high operating cost, small processing capacity, inability to work continuously, and cannot be well applied to on-site industrial production.

The associated minerals in attapulgite ore are mainly quartz, dolomite, etc. Among them, the Mohs hardness of quartz is 7, the specific gravity is 2.22-2.65; the Mohs hardness of dolomite is 3.5-4, and the specific gravity is 2.8-2.9; attapulgite The Mohs hardness of stone is 2-3, and the specific gravity is 2.05-2.30. Attapulgite has lower hardness and lower density.

SUMMARY OF THE INVENTION

The invention provides a method and device for purifying attapulgite clay, so as to realize the purification of attapulgite clay from the physical properties of attapulgite.

In order to achieve the above purpose, the following technical solutions are adopted:

A method for purifying attapulgite clay, comprising the following steps:

Step A, crushing the attapulgite raw ore, adding water to the crushed attapulgite to prepare a suspension, adding it into a mixing bucket, and performing slurry mixing treatment to obtain an attapulgite suspension;

In step B, the attapulgite suspension obtained in step A is fed into the hydrocyclone using a feeding pump, and the materials are evenly fed, and the sorted hydrocyclone underflow is collected, sorted again, and collected twice. The overflow after sorting is used to obtain purified attapulgite clay.

In the step A, the rough attapulgite ore is crushed with a jaw crusher, and the discharge particle size is 25 mm.

In the step A, the mass concentration of the attapulgite suspension is 5-10%.

In the step B, the feeding pressure when the suspension is fed into the hydrocyclone by the feeding pump is 0.10-0.20 MPa.

In the step B, the diameter of the underflow port of the hydrocyclone is 6-10 mm.

A device for realizing the purification method of the attapulgite clay, comprising a stirring tank and a cyclone, wherein:

The stirring barrel is provided with a stirrer, and the stirrer is connected with the stirrer motor arranged outside the stirring barrel;

The upper part of the cyclone is provided with a feeding port, the feeding port is connected with the bottom of the mixing tank through a pipeline, and a feeding pump is arranged in the pipeline, the bottom of the cyclone is connected with an underflow pipe, and the bottom of the underflow pipe is connected with a No. A liquid collection tank, the top of the cyclone is connected with an overflow pipe, the other end of the overflow pipe is connected with a second liquid collection tank, and the bottoms of the first liquid collection tank and the second liquid collection tank are connected to the upper part of the agitator through pipelines .

The bottom of the mixing barrel is provided with a valve.

A sampling port is provided on the pipeline between the feeding pump and the feeding port.

The principle of the present invention is: according to the hydrophilicity and high swelling property of attapulgite, the attapulgite ore is crushed and then added into water, under the action of mechanical force, attapulgite will be rapidly dispersed in water, fully dissociated, and The integrity of the particles will not be damaged, and the purpose of separating attapulgite from gangue minerals is achieved. After slurry conditioning, the attapulgite and gangue minerals are completely separated. During the separation of the hydrocyclone, the gangue minerals with high density and large particle size will flow along the outer swirling direction of the hydrocyclone under the action of centrifugal force. The attapulgite with low density and small particle size will move upward with the internal swirling flow, and finally be discharged from the overflow port as a concentrate product.

Beneficial effects: The present invention starts from the physical properties of attapulgite, attempts to dissociate attapulgite and gangue minerals by crushing and stirring and mixing, and uses hydrocyclone for separation after sufficient dissociation. By adjusting the slurry concentration, feeding pressure, cone ratio of the cyclone and other conditions, it is separated to achieve the effect of purification. Compared with the traditional wet purification method, the hydrocyclone sorting has a large processing capacity and can work continuously. The process is simple and the operation difficulty is low. Non-toxic and non-polluting, it has high application value.

Compared with the prior art, the present invention has the following advantages:

(1) The separation method of hydrocyclone is adopted, compared with the traditional wet separation, the processing capacity is large, the operation is simple, and it can work continuously. (2) The process flow is optimized, and the method of one-time separation and underflow re-selection is adopted to effectively improve the yield of attapulgite concentrate. (3) Through the method of physical sorting, the sorting process does not use any additives, and there is no waste liquid discharge, which is green and environmentally friendly. (4) Attapulgite is a natural clay mineral with abundant reserves and wide sources. The purification method of the present invention has low cost and simple operation, and can be applied on a large scale in industry.

Description of drawings

Fig. 1 is the device structure schematic diagram of the present invention;

In the picture: 1- agitator motor, 2- attapulgite ore, 3- mixing barrel, 4- valve, 5- feeding pump, 6- sampling port, 7- feeding port, 8- overflow pipe, 9- The main body of the cyclone, 10-underflow pipe, 11-agitator, 12-first liquid collection tank, 13-second liquid collection tank;

Fig. 2 is the XRD figure of the attapulgite ore of embodiment 1;

3 is a XRD comparison diagram of the underflow and the overflow after the attapulgite clay of Example 1 is sorted by a hydrocyclone.

Detailed ways

A method for purifying attapulgite clay of the present invention, comprising the following steps:

In step A, the raw attapulgite ore is crushed with a jaw crusher, and the discharge particle size is 25 mm, the crushed attapulgite is mixed with water to prepare a suspension with a mass concentration of 5-10%, and it is added into the mixing barrel, Carry out sizing treatment to obtain attapulgite suspension;

In step B, the attapulgite suspension obtained in step A is fed into the hydrocyclone using the feeding pump, the feeding pressure is 0.10-0.20MPa, the feeding is uniform, and the sorted hydrocyclone is underflowed. Collecting and sorting again, the diameter of the underflow port of the hydrocyclone is 6-10 mm, and the overflow after two sorting is collected to obtain the purified attapulgite clay.

As shown in Figure 2, a purification device for attapulgite clay, comprising a mixing barrel 3 and a cyclone 9, wherein:

An agitator 11 is arranged in the mixing bucket 3 , and the agitator 11 is connected to the agitator motor 1 arranged outside the mixing bucket 3 ; a valve 4 is arranged at the bottom of the mixing bucket 3 .

The upper part of the cyclone 9 is provided with a feeding port 7, and the feeding port 7 is connected with the bottom of the mixing barrel 3 through a pipeline, and a feeding pump 5 is arranged in the pipeline, and the gap between the feeding pump 5 and the feeding port 7 is The pipeline is provided with a sampling port 6; the bottom of the cyclone 9 is connected with an underflow pipe 10, the bottom of the underflow pipe 10 is connected with a first liquid collection tank 12, the top of the cyclone 9 is connected with an overflow pipe 8, and the other end of the overflow pipe 8 is connected A second liquid collection tank 13 is connected, and the bottoms of the first liquid collection tank 12 and the second liquid collection tank 13 are connected to the upper part of the agitator 11 through pipelines.

The present invention will be further described below with reference to specific embodiments.

Example 1

A. Slurry treatment of attapulgite:

The raw attapulgite ore is crushed with a jaw crusher, and the discharge particle size is 25mm. The crushed material and water are prepared into an attapulgite suspension with a mass concentration of 8% in the mixing barrel, and it is allowed to stand for 24 hours. Turn on the mixer switch and start mixing. The speed of the mixer is 1300r/min. After mixing for 1h, it is ready for use.

B, purification of attapulgite:

The attapulgite suspension that has undergone sizing treatment in step A is fed into a hydrocyclone for sorting through a feeding pump, the feeding pressure is 0.15 MPa, the aperture of the underflow port is 6 mm, and all overflow products are collected, The underflow product is returned to the mixing tank for re-selection, and the re-selection overflow product is collected and used as concentrate together with the first-time separation overflow product, and the underflow product is re-selected as tailings, which is the purified attapulgite. The viscosity of the attapulgite raw ore at a pressure of 1Pa was 4.30cP measured by a rotational rheometer, and the viscosity of the sorted attapulgite was 5.88cP, and the colloidal properties of the attapulgite were improved. The elements of the sample were analyzed by X-ray fluorescence spectrometer. The mass fraction of Si in the underflow product was 58.75%, the mass fraction of Mg was 4.82%, and the mass fraction of Al was 12.39%; the mass fraction of Si in the overflow product was 50.91%, and the mass fraction of Mg was 50.91%. The fraction is 6.72%, and the Al mass fraction is 15.96%.

Example 2

A. Slurry treatment of attapulgite:

The raw attapulgite ore is crushed with a jaw crusher, and the discharge particle size is 25mm. The crushed material and water are prepared into a suspension of attapulgite with a mass concentration of 5% in the mixing barrel, and it is allowed to stand for 24 hours. Turn on the mixer switch and start mixing. The speed of the mixer is 1300r/min. After mixing for 1h, it is ready for use.

B, purification of attapulgite:

The attapulgite suspension that has undergone sizing treatment in step A is fed into a hydrocyclone for sorting through a feeding pump, the feeding pressure is 0.20 MPa, the aperture of the underflow port is 8 mm, and all overflow products are collected, The underflow product is returned to the mixing tank for re-selection, and the re-selection overflow product is collected and used as concentrate together with the first-time separation overflow product, and the underflow product is re-selected as tailings, which is the purified attapulgite. Using a rotational rheometer, the viscosity of the attapulgite raw ore at a pressure of 1 Pa was measured to be 4.30 cP, and the viscosity of the sorted attapulgite was 5.32 cP, and the colloidal property of the attapulgite was improved. The elements of the sample were analyzed by X-ray fluorescence spectrometer. The mass fraction of Si in the underflow product was 59.66%, the mass fraction of Mg was 4.68%, and the mass fraction of Al was 11.91%; the mass fraction of Si in the overflow product was 50.72%, and the mass fraction of Mg was 50.72%. The fraction is 6.70%, and the Al mass fraction is 16.04%.

Example 3

A. Slurry treatment of attapulgite:

The raw attapulgite ore is crushed with a jaw crusher, and the discharge particle size is 25mm. The crushed material and water are prepared into an attapulgite suspension with a mass concentration of 8% in the mixing barrel, and it is allowed to stand for 24 hours. Turn on the mixer switch and start mixing. The speed of the mixer is 1300r/min. After mixing for 1h, it is ready for use.

B, purification of attapulgite:

The attapulgite suspension that has undergone sizing treatment in step A is fed into a hydrocyclone for sorting through a feeding pump, the feeding pressure is 0.20 MPa, the aperture of the underflow port is 10 mm, and all overflow products are collected, The underflow product is returned to the mixing tank for re-selection, and the re-selection overflow product is collected and used as concentrate together with the first-time separation overflow product, and the underflow product is re-selected as tailings, which is the purified attapulgite. The viscosity of attapulgite raw ore was 4.30cP when the pressure was 1Pa measured by rotational rheometer, the viscosity of attapulgite after separation was 5.40cP, and the colloidal property of attapulgite was improved. The elements of the sample were analyzed by X-ray fluorescence spectrometer. The mass fraction of Si in the underflow product was 55.75%, the mass fraction of Mg was 5.42%, and the mass fraction of Al was 12.88%; the mass fraction of Si in the overflow product was 50.9%, and the mass fraction of Mg was 50.9%. The fraction is 6.76%, and the Al mass fraction is 15.95%.

The above are only the preferred embodiments of the present invention. It should be pointed out that for those skilled in the art, without departing from the principles of the present invention, several improvements and modifications can be made. It should be regarded as the protection scope of the present invention.

Claims (9)

1. a purification method of attapulgite clay, is characterized in that: comprise the following steps: Step A, crushing the attapulgite raw ore, adding water to the crushed attapulgite to prepare a suspension, adding it into a mixing bucket, and performing slurry mixing treatment to obtain an attapulgite suspension; In step B, the attapulgite suspension obtained in step A is fed into the hydrocyclone using a feeding pump, and the materials are evenly fed, and the sorted hydrocyclone underflow is collected, sorted again, and collected twice. The overflow after sorting is used to obtain purified attapulgite clay. 2 . The method for purifying attapulgite clay according to claim 1 , wherein in the step A, the raw attapulgite ore is crushed with a jaw crusher, and the discharge particle size is less than or equal to 25mm. 3 . 3. The method for purifying attapulgite clay according to claim 1, wherein in the step A, the mass concentration of the attapulgite suspension is 5-10%. 4. The method for purifying attapulgite clay according to claim 1, characterized in that: in the step A, the rotating speed of the mixer is 1300 r/min, and the mixing time is not less than 1 hour. 5. The method for purifying attapulgite clay according to claim 1, characterized in that: in the step B, the feeding pressure when the suspension is fed into the hydrocyclone using a feeding pump is 0.10-0.20 MPa. 6 . The method for purifying attapulgite clay according to claim 1 , wherein in the step B, the aperture of the hydrocyclone underflow port is 6-10 mm. 7 . 7. a device for realizing the purification method of attapulgite clay as claimed in claim 1, is characterized in that: comprises mixing barrel (3) and cyclone (9), wherein: An agitator (11) is arranged in the mixing barrel (3), and the agitator (11) is connected with the agitator motor (1) arranged outside the mixing barrel (3); The upper part of the cyclone (9) is provided with a feeding port (7), and the feeding port (7) is connected with the bottom of the mixing barrel (3) through a pipeline, and a feeding pump (5) is arranged in the pipeline, The bottom of the cyclone (9) is connected with an underflow pipe (10), the bottom of the underflow pipe (10) is connected with a first liquid collecting tank (12), and the top of the cyclone (9) is connected with an overflow pipe (8). The other end of the pipe (8) is connected with a second liquid collection tank (13), and the bottoms of the first liquid collection tank (12) and the second liquid collection tank (13) are connected to the upper part of the agitator (11) through pipelines. 8. The device according to claim 7, characterized in that: a valve (4) is provided at the bottom of the mixing barrel (3). 9 . The device according to claim 7 , wherein a sampling port ( 6 ) is provided on the pipeline between the feeding pump ( 5 ) and the feeding port ( 7 ). 10 .

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