Method for extracting sporopollen from gypsum layer and application

Abstract

The invention discloses a method for extracting sporopollen from a gypsum layer and application. The method comprises the following steps: selecting the third gypsum layer sediment of the basin; drying and grinding the gypsum layer sediment, mixing the gypsum layer sediment with ammonium carbonate and water to carry out cation exchange reaction, and then adding hydrochloric acid to carry out reaction to obtain a first product; adding hydrofluoric acid into the first product and reacting to obtain a second product; and under the ultrasonic condition, enabling the second product to pass through a screen, and then collecting the product on the screen, thereby realizing the extraction of the sporopollen in the gypsum layer. The method for extracting the sporopollen from the gypsum layer of the salt lake sediment is a great innovation, the traditional sporopollen is mainly separated and extracted from a mudstone layer and a peat layer, and the sporopollen is extracted from the gypsum layer for the first time; meanwhile, the process of obtaining the agaricus bisporus is simple to operate, and the solid waste discharge amount is small.

Description

Technical Field

[0001] The invention belongs to the field of separation technology, and particularly relates to a method for extracting sporopollen from a gypsum layer and application thereof. Background Art

[0002] The entire plant kingdom can generally be divided into two categories: spore plants and seed plants. The former, such as mosses and ferns, reproduce by spores; the latter, such as gymnosperms and angiosperms, reproduce by seeds. Certain plants produce specific types of spores or pollen, while different plants produce different types of spores or pollen. Throughout geological history, plants have evolved in response to changing natural and geographical conditions, from low-level to high-level, from simple to complex. Certain plants growing at certain times produced unique forms of spores or pollen. Consequently, the spore and pollen assemblages of each era are unique.

[0003] Due to the development of the national economy, there is an urgent need to solve some problems in geological exploration, so pollen analysis is currently the most widely used in geology. The scope of application can be roughly divided into: 1. Identification of stratigraphic age. Plants in different historical periods are different, and the spores or pollen produced are also different. Therefore, pollen analysis methods can be used to identify the age of strata; 2. Comparison of strata (including coal seam comparison). If roughly similar pollen combinations are found in two sedimentary layers in a certain area, it can be considered that the two layers containing similar combinations were basically deposited at the same time, and therefore can be compared. In addition, pollen analysis is widely used in geography, paleoclimatology, and botany, and has also been studied in medicine and agriculture.

[0004] Pollen and rock-forming materials are mixed in the sediments, and pollen buried in the rock is not easy to study under a light-transmitting biological microscope. Therefore, pollen needs to be separated from the rock. Due to the light transmission of pollen itself, it can be observed under a microscope. Generally speaking, it is easier to extract pollen from rocks with a high organic content, such as peat, coal, black and gray-black shales, mudstones, and siltstones. Red and yellow rocks generally do not contain pollen. Treatment methods can be divided into two categories: one is to use chemical methods to dissolve rock particles, leaving pollen (such as the hydrofluoric acid method for treating rocks and the Atman method for treating peat); the other is a combination of chemical and physical methods, first separating pollen from rock particles, and then concentrating the pollen according to different specific gravities (such as Grichuk's separation method).

[0005] The salt lake evaporite sequence (carbonate → sulfate → chloride) indicates the stage of brine concentration and locates the enrichment layers of minerals such as potassium salt, lithium, and boron (such as the potassium salt deposits in the Qarhan Salt Lake in the Qaidam Basin). Salt lake sediments are an important carrier of strategic minerals, and paleoenvironmental research can provide key clues for resource prediction. In the study of salt lake paleoenvironment, palynology not only serves resource exploration (stratigraphic dating, mineral prediction), but also restores the detailed evolution of ancient ecosystems through vegetation-climate-hydrological coupling analysis. Its data can be cross-validated with geochemical and sedimentological indicators to construct a multi-dimensional environmental model. In the future, combined with new technologies (such as ancient DNA, AI) and multidisciplinary integration, palynology will play a more core role in decoding the "salt lake code" and provide scientific support from a deep time perspective for responding to contemporary climate change and resource management.

[0006] The depositional age of salt deposits is crucial for accurately understanding basin evolution, the timing of fluid migration and trap formation, and the initiation of salt movement. Similarly, determining the age of salt deposits is crucial for basin analysis, forward modeling, and tectonic reconstruction. Salt deposit ages are typically estimated based on the ages of underlying and overlying strata. This method can provide a rough estimate of depositional age, but if the salt deposit is mobile, its boundary strata often mark the stage of salt movement rather than the original depositional age, which can lead to biased estimates. Furthermore, these methods cannot accurately determine the time span of salt deposition. Previous studies have primarily extracted pollen from mudstone and argillaceous siltstone layers, but have not examined pollen from salt deposits (halite and gypsum layers). Due to the insolubility of gypsum, current pollen extraction methods are primarily targeted at mudstone and peat layers and are incapable of extracting pollen from salt lake sediments (halite and gypsum layers). To date, no effective method for extracting pollen from gypsum layers exists. Summary of the Invention

[0007] The main purpose of the present invention is to provide a method for extracting sporopollen from a gypsum layer and its application, so as to overcome the shortcomings of the prior art.

[0008] To achieve the aforementioned object of the invention, the technical solutions adopted by the present invention include:

[0009] An embodiment of the present invention provides a method for extracting pollen from a gypsum layer, comprising:

[0010] The Tertiary gypsum sediments of the basin were selected;

[0011] The gypsum layer sediment is dried and crushed, and then mixed with ammonium carbonate and water to perform a cation exchange reaction, and then hydrochloric acid is added to react to obtain a first product;

[0012] adding hydrofluoric acid to the first product and reacting to obtain a second product;

[0013] And, under ultrasonic conditions, the second product is passed through a sieve, and then the product on the sieve is collected, thereby achieving the extraction of spore pollen in the gypsum layer.

[0014] The embodiment of the present invention also provides the application of the aforementioned method for extracting pollen from a gypsum layer in geological exploration.

[0015] Compared with the prior art, the present invention has the following beneficial effects:

[0016] (1) The invention extracts pollen from the gypsum layer in the salt lake sediment, which is a major innovation of the invention. Traditional pollen extraction is mainly separated and extracted from mudstone layers and peat layers. Extracting pollen from the gypsum layer is the first time.

[0017] (2) The process of obtaining spore pollen in the present invention is simple to operate and produces little solid waste. DETAILED DESCRIPTION

[0018] In view of the shortcomings of the prior art, the inventors of this case, after long-term research and extensive practice, have proposed the technical solution of the present invention. The technical solution of the present invention will be clearly and completely described below. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making any creative effort shall fall within the scope of protection of the present invention.

[0019] Specifically, as one aspect of the technical solution of the present invention, a method for extracting pollen from a gypsum layer includes:

[0020] The Tertiary gypsum sediments of the basin were selected;

[0021] The gypsum layer sediment is dried and crushed, and then mixed with ammonium carbonate and water to perform a cation exchange reaction, and then hydrochloric acid is added to react to obtain a first product;

[0022] adding hydrofluoric acid to the first product and reacting to obtain a second product;

[0023] And, under ultrasonic conditions, the second product is passed through a sieve, and then the product on the sieve is collected, thereby achieving the extraction of spore pollen in the gypsum layer.

[0024] In some preferred embodiments, the basin includes any one or more combinations of the Nangqian Basin, Xining Basin, Tuotuo River Basin, Hoh Xil Basin, and Xia Laxiu Basin, but is not limited thereto.

[0025] In some preferred embodiments, the method specifically includes: drying the gypsum layer deposit at 35-45° C. for 0.5-1.5 h.

[0026] Furthermore, the gypsum layer deposit was dried at 40° C. for 1.0 h.

[0027] In some preferred embodiments, the method specifically comprises: grinding the product obtained by drying, so that the particle size of the product obtained by the grinding is at least 1 to 3 mm.

[0028] In some preferred embodiments, the method specifically includes: mixing the product obtained by the crushing treatment with ammonium carbonate and water to perform a cation exchange reaction, then adding hydrochloric acid to remove carbonate until no bubbles are generated, then washing with water until neutral, and collecting solids to obtain the first product.

[0029] Furthermore, the product obtained by the crushing treatment is mixed with ammonium carbonate and water for a cation exchange reaction, and then hydrochloric acid is added to fully react. After standing for 7 hours, the supernatant is removed, and then water is added and continued to stand for 7 hours, and the supernatant is removed again (this is the process of washing the sample to neutrality). This step of adding water is repeated at least four times, washing to neutrality, and the supernatant is removed for the last time, leaving the solid substance at the bottom of the beaker as the first product, waiting for the addition of hydrofluoric acid.

[0030] Furthermore, the ratio of the product obtained by the crushing process, ammonium carbonate and water is 50g:100g:500mL.

[0031] Among them, ammonium carbonate parameters: analytical grade (AR), content (calculated as NH4), W / %>40.0.

[0032] Furthermore, the concentration of the hydrochloric acid is 37 wt%.

[0033] In some preferred embodiments, the method specifically comprises: adding hydrofluoric acid to the first product and reacting at room temperature for 24 hours, then washing with water until neutral, and collecting the solid to obtain the second product.

[0034] Furthermore, hydrofluoric acid was added to the first product until it fully reacted, and then it was allowed to stand for 7 hours. The supernatant was removed, and then water was added and the mixture was allowed to stand for another 7 hours. The supernatant was then removed (this was the process of washing the sample to neutrality). This step of adding water was repeated at least four times until it was neutral. The supernatant was removed for the last time, leaving the solid matter at the bottom of the beaker as the second product, which was awaiting ultrasonic cleaning.

[0035] Furthermore, the volume ratio of the first product to hydrofluoric acid is 1:3.

[0036] In some preferred embodiments, the method specifically includes: placing a sieve with a pore size of 10 μm in an ultrasonic device, then pouring the second product into the sieve and collecting the product on the sieve, thereby achieving the extraction of spore pollen in the gypsum layer.

[0037] Specifically, the mesh is placed in ultrasound, water is added in the ultrasound, and the second product is poured into the mesh.

[0038] In some preferred embodiments, the ultrasonic treatment uses a power of 35 to 45 W, an ultrasonic frequency of 35 to 45 KHz, and a time of 5 to 15 minutes.

[0039] Furthermore, the ultrasonic treatment adopts a power of 40W, an ultrasonic frequency of 40KHz, and a time of 10 minutes.

[0040] Currently, all potash in my country comes from modern salt lake brines from the Quaternary. Potash resources in salt lakes primarily exist in liquid form, and their total reserves are only a few hundred million tons, far short of my country's current demand. By the end of the last century, exploration of potash resources in my country's salt lakes had essentially been completed, and it is now difficult to find large-scale potash deposits in my country's salt lakes. The greatest constraint on the development of the potash fertilizer industry is the lack of reserve potash resources, and the active search for new potash deposits is urgent. The Mesozoic and Cenozoic salt basins in southern Qinghai possess several favorable conditions for potash formation, as follows:

[0041] There are several Mesozoic-Cenozoic salt basins in southern Qinghai, such as the Tuotuo River and Hoh Xil Basins in western Yushu, and the Nangqian Basin and Xialaxiu Basin in eastern Yushu. The existence of these basins provides a favorable place for salt (potassium) formation. Regional geological survey data and our research data show that there are many salt-bearing strata distributed in the salt basins in southern Qinghai, and at the same time, insoluble gypsum layers are widely distributed on the surface. The present invention selects the gypsum layer of the Nangqian Basin.

[0042] (1) First, dry the gypsum sediment, crush it, and weigh 50 grams into a beaker;

[0043] (2) Then add 100 g of ammonium carbonate and 500 ml of deionized water and stir. The specific reaction is: the cation exchange of calcium sulfate (gypsum) and ammonium carbonate (Ca 2+ With NH4 + Interchange), producing less soluble calcium carbonate (CaCO3) precipitate and soluble ammonium sulfate ((NH4)2SO4);

[0044] (3) Slowly inject 37 wt% hydrochloric acid (to remove carbonates) into the beaker until no bubbles are generated. Finally, wash with water until neutral (add water and let it stand for 7 hours, then remove the supernatant with a plastic tube, repeat four times), and collect the solids at the bottom;

[0045] (4) Add an appropriate amount of hydrofluoric acid (to remove silicates) and allow to react for 24 hours. Shake once every hour (to facilitate complete reaction). Then wash with water until neutral (add water and let stand for 7 hours, then remove the supernatant with a plastic tube. Repeat four times). Collect the solids at the bottom.

[0046] (5) Use a 10 μm sieve to place an ultrasonic filter, and pass the solids washed to the neutral bottom through the sieve. Finally, collect the material on the sieve into a 15 ml microcentrifuge tube for identification.

[0047] Another aspect of the embodiments of the present invention further provides the application of the aforementioned method for extracting pollen from a gypsum layer in geological exploration.

[0048] The technical solution of the present invention is further described in detail below in conjunction with several preferred embodiments. This embodiment is implemented on the premise of the technical solution of the invention, and provides a detailed implementation method and specific operation process, but the protection scope of the present invention is not limited to the following embodiments.

[0049] Unless otherwise specified, the experimental materials used in the following examples can be purchased from conventional biochemical reagent companies.

[0050] Example 1

[0051] The present invention selects the Tertiary gypsum layer (gypsum containing mud and sand) in the Nangqian Basin.

[0052] (1) First, dry the gypsum sediment (dry at 40°C for 1.0 h), crush it, and weigh 50 g into a beaker;

[0053] (2) Then add 100 g of ammonium carbonate and 500 ml of deionized water and stir thoroughly. The specific reaction is: cation exchange of calcium sulfate (gypsum) with ammonium carbonate (Ca 2+ With NH4 + Interchange), producing less soluble calcium carbonate (CaCO3) precipitate and soluble ammonium sulfate ((NH4)2SO4);

[0054] (3) Slowly inject 37 wt% hydrochloric acid (to remove carbonates) into the beaker until no bubbles are generated. Finally, wash with water until neutral (add water and let it stand for 7 hours, then remove the supernatant with a plastic tube, repeat four times), and collect the solids at the bottom;

[0055] (4) Add an appropriate amount of hydrofluoric acid (to remove silicates) and react at room temperature for 24 hours. Shake once every hour (to facilitate complete reaction). Then wash with water until neutral (add water and let it stand for 7 hours. Use a plastic tube to extract the supernatant. Repeat four times). Collect the solids at the bottom.

[0056] (5) Ultrasonic waves (ultrasonic treatment power of 40 W, ultrasonic frequency of 40 kHz, and time of 10 min) were placed through a 10 μm sieve to pass the solids washed to the neutral bottom through the sieve. The material on the sieve was collected into a 15 ml microcentrifuge tube and identified under a microscope, where a large amount of pollen was found.

[0057] Example 2

[0058] The present invention selects the Tertiary gypsum layer (gypsum containing mud and sand) in the Xining Basin.

[0059] (1) First, dry the gypsum sediment (dry at 40°C for 1.0 h), crush it, and weigh 50 g into a beaker;

[0060] (2) Then add 100 g of ammonium carbonate and 500 ml of deionized water and stir thoroughly. The specific reaction is: cation exchange of calcium sulfate (gypsum) with ammonium carbonate (Ca 2+ With NH4 + Interchange), producing less soluble calcium carbonate (CaCO3) precipitate and soluble ammonium sulfate ((NH4)2SO4);

[0061] (3) Slowly inject 37 wt% hydrochloric acid (to remove carbonates) into the beaker until no bubbles are generated. Finally, wash with water until neutral (add water and let it stand for 7 hours, then remove the supernatant with a plastic tube, repeat four times), and collect the solids at the bottom;

[0062] (4) Add an appropriate amount of hydrofluoric acid (to remove silicates) and react at room temperature for 24 hours. Shake once every hour (to facilitate complete reaction). Then wash with water until neutral (add water and let it stand for 7 hours. Use a plastic tube to extract the supernatant. Repeat four times). Collect the solids at the bottom.

[0063] (5) Ultrasonic waves (ultrasonic treatment power of 40 W, ultrasonic frequency of 40 kHz, and time of 10 min) were placed through a 10 μm sieve to pass the solids washed to the neutral bottom through the sieve. The material on the sieve was collected into a 15 ml microcentrifuge tube and identified under a microscope, where a large amount of pollen was found.

[0064] In addition, the inventors of this case also referred to the aforementioned embodiments and conducted experiments using other raw materials, process operations, and process conditions described in this specification, and obtained relatively ideal results.

[0065] It should be understood that the technical solution of the present invention is not limited to the above-mentioned specific implementation cases. Any technical variations made according to the technical solution of the present invention without departing from the scope of protection of the purpose of the present invention and the claims shall fall within the scope of protection of the present invention.

Claims

1. A method for extracting pollen from a gypsum layer, characterized in that: include: The Tertiary gypsum sediments of the basin were selected; The gypsum layer sediment is dried and crushed, and then mixed with ammonium carbonate and water to perform a cation exchange reaction, and then hydrochloric acid is added to react to obtain a first product; adding hydrofluoric acid to the first product and reacting to obtain a second product; And, under ultrasonic conditions, the second product is passed through a sieve, and then the product on the sieve is collected, thereby achieving the extraction of spore pollen in the gypsum layer.

2. The method according to claim 1, wherein: The basins include any one or more combinations of the Nangqian Basin, Xining Basin, Tuotuo River Basin, Hoh Xil Basin, and Xia Laxiu Basin.

3. The method according to claim 1, characterized in that Specifically include: Drying the gypsum layer sediment at 35-45° C. for 0.5-1.5 h; And / or, the method comprises: grinding the product obtained by drying, so that the particle size of the product obtained by the grinding is at least 1 to 3 mm.

4. The method according to claim 1, wherein Specifically include: The product obtained by the crushing treatment is mixed with ammonium carbonate and water to carry out a cation exchange reaction, and then hydrochloric acid is added to remove carbonate until no bubbles are generated. The product is then washed with water until neutral, and the solid matter is collected to obtain the first product.

5. The method according to claim 4, characterized in that: The ratio of the product obtained by the crushing process, ammonium carbonate and water is 50g:100g:500mL; And / or, the concentration of the hydrochloric acid is 37 wt %.

6. The method according to claim 1, characterized in that Specifically include: Hydrofluoric acid was added to the first product and reacted at room temperature for 24 h, then washed with water until neutral, and the solid was collected to obtain the second product.

7. The method according to claim 6, characterized in that: The volume ratio of the first product to hydrofluoric acid is 1:

3.

8. The method according to claim 1, characterized in that Specifically include: A sieve with a pore size of 10 μm is placed in an ultrasonic device, and then the second product is poured into the sieve and the product on the sieve is collected, thereby achieving the extraction of spore pollen in the gypsum layer.

9. The method according to claim 1, wherein: The ultrasonic treatment adopts a power of 35 to 45 W, an ultrasonic frequency of 35 to 45 KHz, and a time of 5 to 15 minutes.

10. the application of the method for extracting pollen from gypsum layer described in any one among claim 1-9 in geological prospecting.