Solid adsorbent for urine purification, preparation method and urine purification device

Abstract

The invention discloses a solid adsorbent for urine purification. The solid adsorbent comprises diatomite which is sequentially subjected to purification, activation treatment, alkalization treatment, anionic surfactant treatment and baking activation treatment; the activation treatment comprises baking in a first specific temperature range for a first specific time range, the alkalization comprises placing diatomite subjected to activation treatment and purification in an environment with a pH value of 7-11, and the anionic surface treatment comprises adding a treatment solution formed by an anionic surfactant into the diatomite subjected to the alkalization treatment and carrying out full stirring, uniform mixing, standing and centrifugation. Removing the supernatant and collecting the precipitate; the baking and activating treatment refers to baking in a second specific temperature range for a second specific duration range. The invention further discloses a preparation method of the solid adsorbent and a urine purification device, the urine purification device comprises a bearing container, the bearing container comprises a pipe body, and the solid adsorbent for urine purification is filled in the pipe body; the top of the tube body is provided with a liquid injection port and a plug head; a liquid dropping opening and a lower plug cap are arranged below; filter paper is laid at the bottom of the pipe body.

Description

Technical Field

[0001] The invention relates to the technical field of removing interferences in urine, and in particular to a solid adsorbent for urine purification, a preparation method and a urine purification device. Background Art

[0002] Iodine has the function of maintaining thyroid function, and iodine is a necessary nutrient for the body to produce thyroid hormones. Iodine is very important for maintaining normal thyroid function and growth and development. Iodine can promote the synthesis of thyroid hormones, which can promote body development and protein synthesis. Thyroid hormones have the effect of promoting the development of bones, reproductive organs and brain.

[0003] Iodine in the human body is mainly excreted through urine. Urine iodine testing is a common method for clinical diagnosis of low iodine and high iodine, and is also one of the main methods for evaluating iodine nutritional levels.

[0004] The components of urine are water, urea (molecular formula CH4N2O), uric acid (molecular formula C5H4N4O3), creatinine (molecular formula C4H7N3O), protein (biological macromolecules composed of one or more polypeptide chains), glucose (molecular formula C6H12O6), inorganic salts and electrolytes, etc. Since the content of iodine in urine is extremely small (normal value 100-300ug / L), other components in urine will interfere with the test results and affect the recovery rate of urine iodine, making it impossible to accurately detect its content. The existing urine iodine determination technology at home and abroad mainly uses urine iodine determination kits, and the corresponding urine purification device is a titration container with a selective specific adsorbent. The selective specific adsorbent is an adsorbent composed of 0.2-1g of purified activated carbon and 100-1000ug iodine adsorption antagonist, which is used to specifically adsorb interfering substances in urine. The purified activated carbon is soaked in buffer and the iodine adsorption antagonist is baked at 70-250℃ for 4-72 hours for activation. However, this urine purification device can only adsorb some interferences in urine, and the recovery rate of urine iodine is low (that is, some doses of iodine in urine are lost during the purification process), which still has a very large impact on the test results, directly affecting the diagnosis and treatment of the disease, and causing misdiagnosis and missed diagnosis. Summary of the invention

[0005] The purpose of the present invention is to overcome the defects of the prior art and to address the problems in the related art. A solid adsorbent for urine purification, a preparation method and a urine purification device are provided. The solid adsorbent is treated with diatomaceous earth and alkali and then baked and activated with an anionic surfactant. The solid adsorbent is made by alkalizing diatomaceous earth and anionic surfactant (soap) and then activated to remove most of the interferences in urine. The solid adsorbent is used in a urine purification device to remove interferences (urea, uric acid, creatinine, glucose, protein). The recovery test using national standard urine iodine substances can reach 95%, making the urine iodine detection result accurate, which provides great help for clinical precision diagnosis and treatment.

[0006] The first aspect of the present invention is to provide a solid adsorbent for urine purification, comprising: diatomaceous earth that has been purified, activated, alkalized, treated with anionic surfactants and baked for activation in sequence; wherein the activation treatment comprises baking the diatomaceous earth within a first specific temperature range for a first specific time range, the alkalization comprises placing the diatomaceous earth purified by the activation treatment in an environment with a pH value of 7-11, the anionic surface treatment comprises adding a treatment solution formed by the anionic surfactant to the diatomaceous earth that has been alkalized, and stirring, mixing, standing and centrifuging the treatment solution, discarding the supernatant and collecting the precipitate; the baking activation treatment comprises baking the diatomaceous earth treated with the anionic surfactant within a second specific temperature range for a second specific time range.

[0007] The second aspect of the present invention is to provide a method for preparing a solid adsorbent for urine purification, comprising: S1, purifying diatomite, comprising: adopting a single purification method or a combined purification method; the single purification method comprises: a scrubbing method, an acid leaching method, a roasting method, a magnetic separation method, a thermal sedimentation method or a thermal flotation method; the combined purification method comprises: a scrubbing-acid leaching method, a water washing-roasting method, a roasting-acid leaching method, a roasting-alkali leaching method, a thermal flotation-magnetic separation-acid boiling method and a scrubbing-microwave-acid leaching method; S2, activating the purified diatomaceous earth, including: baking the purified diatomaceous earth at a first specific temperature range for a first specific time range for activation treatment; S3, alkalizing the activated diatomaceous earth, including: placing the activated and purified diatomaceous earth in an environment with a pH value of 7-11; S4, treating the alkalized diatomaceous earth with an anionic surfactant; S5, baking the diatomaceous earth treated with the anionic surfactant within a second specific temperature range and a second specific time range to perform activation treatment, and forming the solid adsorbent product after the activation treatment.

[0008] Preferably, the S1 comprises: S11, taking a certain amount of diatomaceous earth and soaking it for a certain period of time; S12, adding a certain concentration and a certain amount of sodium hydroxide as a dispersant to the soaked diatomite, so that the slurry concentration reaches 40%; S13, stirring and scrubbing the slurry to separate the debris minerals, clay minerals and diatoms, and precipitating sand-grade coarse soil, suspended clay and selected diatomaceous earth respectively, and by continuous scrubbing, the debris minerals and clay minerals are removed, the diatoms are relatively enriched, the silicon dioxide content is increased, and the aluminum oxide and iron oxide contents are reduced; S14, taking the diatomaceous earth that has been scrubbed 5-10 times and placing it in a centrifuge for centrifugation, discarding the supernatant after centrifugation and collecting the purified diatomaceous earth precipitate.

[0009] Preferably, the first specific temperature range is 100-300°C.

[0010] Preferably, the first specific duration ranges from 8 to 72 hours.

[0011] Preferably, S4 includes: S41, adding a treatment solution formed by the anionic surfactant to the alkalized diatomaceous earth; S42, after sufficient stirring, mixing, standing and centrifugation, the supernatant is discarded and the precipitate is collected.

[0012] Preferably, the anionic surfactant includes, but is not limited to, one or more of the following substances: soap, alkylbenzene sulfonate, alkyl sulfonate ester salt, alkyl sulfonate, alkyl sulfate, fluorinated fatty acid salt, polysiloxane and fatty alcohol sulfate.

[0013] Preferably, the standing time is 4-36 hours; the centrifugation is performed by placing the mixture in a centrifuge, the centrifugal speed is 2000-3000 rpm, and the centrifugal time is 30-50 min.

[0014] Preferably, S5 comprises: baking the precipitate collected in S42 in an electric constant temperature forced air drying oven at 100-300° C. for 8-72 hours for activation treatment, and the product prepared is a solid adsorbent finished product.

[0015] The third aspect of the present invention is to provide a urine purification device, comprising a carrying container, the carrying container comprising a tube body (3), the solid adsorbent for urine purification according to the first aspect of the present invention being loaded inside the tube body (3); a liquid injection port (2) is arranged at the top of the tube body (3), a plugging cap head (1) for blocking the liquid injection port (2) is arranged above the liquid injection port (2); a dripping port (4) is arranged below the tube body (3), a lower plugging cap (5) for blocking the lower tip of the dripping port (4) is arranged below the dripping port (4); the diameter of one end of the dripping port (4) connected to the tube body (3) is larger than the diameter of one end connected to the lower plugging cap (5); a filter paper (10) is laid at the bottom of the tube body, the solid adsorbent is placed on the filter paper (10) and is in liquid communication with an inlet end with a larger diameter in the dripping port (4), so as to filter and purify urine flowing to the dripping port (4) through the tube body.

[0016] Beneficial effects of the adsorbent, preparation method and urine purification device of the present invention: The interference substances in urine are removed by alkalization of diatomaceous earth and activation with anionic surfactants. The solid adsorbent is treated with diatomaceous earth and alkali and then baked with anionic surfactants for activation. The solid adsorbent made by alkalization of diatomaceous earth and anionic surfactants (soap) can remove most of the interference substances in urine. The use of this solid adsorbent in the urine purification device can remove interference substances (urea, uric acid, creatinine, glucose, protein). The recovery test using national standard urine iodine substances can reach 95%, making the urine iodine test results accurate, providing great help for clinical precision diagnosis and treatment. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the related technologies, the drawings required for use in the specific embodiments or the related technical descriptions will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0018] Figure 1 The present invention is a schematic flow chart of a method for preparing a solid adsorbent for urine purification according to an embodiment of the present invention.

[0019] Figure 2 A schematic flow chart of step S1 in a method for preparing a solid adsorbent for urine purification according to an embodiment of the present invention. Figure 3 The figure is a schematic flow chart of step S4 in the method for preparing a solid adsorbent for urine purification provided in an embodiment of the present invention.

[0020] Figure 4 The figure is a schematic diagram of the structure of a urine purification device provided according to an embodiment of the present invention. DETAILED DESCRIPTION

[0021] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0022] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.

[0023] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0024] The term "about" is used herein in conjunction with numerical values ​​to include the normal variation in measurements expected by those skilled in the art and should be understood to have the same meaning as "approximately" and to cover the typical margin of error, eg, ±5% of the stated value.

[0025] Terms such as "a," "an," and "the" are not intended to refer to only a singular entity, but include the general class that may be illustrated using a specific example.

[0026] Unless otherwise indicated, any amount (eg, concentration) of a component in a composition given as a percentage (%) refers to the weight percent per volume. Embodiment 1

[0027] The present embodiment provides a solid adsorbent for urine purification, comprising: diatomaceous earth that has been subjected to purification, activation treatment, alkalization treatment, anionic surfactant treatment and baking activation treatment in sequence; wherein the activation treatment comprises baking the diatomaceous earth within a first specific temperature range for a first specific time range, the alkalization comprises placing the diatomaceous earth purified by the activation treatment in an environment with a pH value of 7-11, the anionic surface treatment comprises adding a treatment solution formed by the anionic surfactant to the diatomaceous earth subjected to the alkalization treatment, and stirring, mixing, standing and centrifuging the treatment solution, discarding the supernatant and collecting the precipitate; the baking activation treatment comprises baking the diatomaceous earth treated with the anionic surfactant within a second specific temperature range for a second specific time range.

[0028] Working principle of solid adsorbents for urine purification: 1. Process of removing interfering substances (urea, uric acid, creatinine, glucose, protein) in urine: (1) Urea: Urea is easily soluble in water and can be hydrolyzed to produce ammonia and carbon dioxide under the action of acid, alkali, and enzyme (acid and alkali need to be heated). Urine is added to the interference removal device, and the sodium hydroxide on the diatomaceous earth reacts with it, so it does not affect the detection of iodine in urine. The chemical formula of urea is CO(NH2)2.

[0029] CO(NH2)2+NaOH→Na2CO3+2NH3+H2O; (2) Uric acid: Uric acid is the main metabolite of birds and reptiles. It is slightly soluble in water and easily forms crystals. The main product in normal human urine is urea, which contains a small amount of uric acid. The sodium hydroxide in diatomaceous earth will not affect the detection of iodine in urine. The chemical formula of uric acid is C5H4N4O3.

[0030] C5H4N4O3+NaOH→Na2CO3+2NH3+H2O; (3) Creatinine: Creatinine is a compound produced during the energy production process of muscles. It is metabolized by creatine phosphate. Normal kidney function can filter and excrete creatinine in the blood. Therefore, the level of creatinine in the blood reflects the filtering function of the kidneys and is an indicator of kidney function. Creatinine levels are affected by many factors, including age, race, gender and body shape. Blood creatinine may increase or decrease in different diseases and physiological conditions. The chemical formula of creatinine is C4H7N3O.

[0031] C5H4N4O3+NaOH→Na2CO3+2NH3+H2O; (4) Glucose: It is the most widely distributed monosaccharide in nature. Glucose contains five hydroxyl groups and one aldehyde group, and has the properties of polyols and aldehydes. It is easy to decompose when heated under alkaline conditions; when urine is added to the urine purification device, the sodium hydroxide in diatomaceous earth is alkaline and decomposes it without affecting the detection of iodine in urine. The chemical formula of glucose is C6H 12 O6.

[0032] C6H 12 O6+NaOH→C6H 11 O6Na+H2O (5) Protein: The proteins in urine include immunoglobulin, albumin, and retinol binding protein. When urine is added to the interference removal device, the sodium hydroxide and silanol on the diatomaceous earth change the internal structure and properties of the protein, causing it to denature and coagulate. This coagulation is irreversible. The filter paper at the bottom of the device prevents it from filtering out, so it does not affect the detection of iodine in urine. The chemical formula of protein is Pr.

[0033] Pr+NaOH→precipitate→water (6) Iodine: The chemical properties of iodine are not as active as those of the same family elements F2, Cl2, and Br2. Iodine has the lowest solubility in water and is only slightly soluble in water, with a solubility of 0.029g / 100g water. I2 can undergo self-oxidation-reduction reaction under alkaline conditions to generate iodate IO3 - With iodide ion I - : 3I2+6OH - →5I - +IO3 - +3H2O This is due to the absence of hypoiodite IO in the solution. - At any temperature, IO - Both undergo rapid self-oxidation-reduction reactions to generate I - and io3 - Therefore, iodine in urine can be detected without being affected.

[0034] (ii) Diatomaceous earth also has the properties of strong adsorption capacity, low thermal conductivity and good chemical stability. Embodiment 2

[0035] like Figure 1 As shown, this embodiment provides a method for preparing a solid adsorbent for urine purification, comprising: S1, purifying diatomaceous earth, comprising: using a single purification method or a combined purification method.

[0036] Diatoms are a type of single-celled algae that are very small, generally 1m to a few mm in size. When this aquatic plant dies, its remains are deposited in the ocean or lake to form diatomaceous earth. The main component of diatomaceous earth is SiO, which exists in the form of SiO·nH20. It also contains a small amount of Al, Fe, Ca, Mg, Na, K, P, etc., and some metal impurities such as Cr and Ba.

[0037] The single purification method comprises: (1) Scrubbing method: Appropriate scrubbing can break up and disperse the raw material particles without destroying the diatom shells. Clay and other mineral impurities fixed on the diatom shells are separated by scrubbing. After classification, clay and other mineral impurities are removed, thereby increasing the SiO2 content. The more scrubbing times, the better the selection effect, and the higher the SiO2 content of the diatomite.

[0038] (2) Acid leaching: Acid leaching generally uses a mixture of hydrofluoric acid and sulfuric acid. The strong acid dissolves impurities such as A12O3, Fe2O3, CaO, and MgO in diatomite to form salts. Turkish diatomite was purified by hydrochloric acid leaching. It was found that as the acid concentration and leaching time increased, hydrochloric acid dissolved impurities such as A12O3, Fe2O3, CaO, and MgO while also dissolving a certain amount of amorphous SiO2, and the dissolution of SiO2 was affected by the presence of alkali metal elements. Acid leaching can not only improve the purity of diatomite, but also reduce the density of diatomite, increase the pore volume and specific surface area, and significantly improve the pore structure. The diatomite obtained by acid leaching is a high-quality raw material for deep-processing products, and the acid solution can be recycled. However, when this method is used to treat diatomite, the amount of acid and water used is very large, and the cost is relatively high.

[0039] (3) Calcination method: The calcination method is mainly used for the beneficiation and purification of high ignition loss diatomite. When the calcination temperature is 600-800℃, the SiO2 content can be significantly increased due to the volatilization of organic matter, while the pore size increases and the surface acid strength increases. The specific surface area reaches the maximum when calcined at 450℃, and the diatom shell will be destroyed when the calcination temperature reaches above 900℃.

[0040] In addition, there are magnetic separation, thermal sedimentation, thermal flotation, etc., and the combined purification method is preferably used.

[0041] The combined purification method comprises: (1) Scrubbing-acid leaching: Low-grade diatomite is purified by scrubbing and acid leaching. The mineral impurities mixed in the diatomite are effectively removed by scrubbing. After three scrubbings, the SiO2 content increases by 13%. The clay impurities inside the diatomite structure are mainly removed by sulfuric acid pickling. After two picklings, the SiO2 content increases by nearly 5%. After purification, the SiO content of the diatomite increases from 70.18% to 87.13%.

[0042] (2) Water washing and roasting: The water washing and roasting process is used to purify the low-grade diatomite with high calcination loss in Inner Mongolia. The quartz, feldspar and clay impurities are removed by water washing, and the organic matter is removed by roasting at 600℃. The number of water washings, water washing temperature, amount of dispersant and roasting temperature are tested. Finally, the SiO2 content in the diatomite is increased from 64.22% to 82.98%.

[0043] (3) Calcination-acid leaching: A roasting-acid leaching purification test was conducted on diatomite from a company in Jilin, and a diatomite with a SiO content of more than 90% was obtained. The study found that below 450°C, the specific surface area of ​​diatomite increased with the increase of roasting temperature. After exceeding 450°C, the specific surface area decreased with the increase of roasting temperature. The appropriate concentration of sulfuric acid was 72%. Through test analysis, it was found that after the original diatomite was purified, most of the impurities were removed, the porosity became better, the specific surface area increased, and the adsorption performance increased. Turkish diatomite was purified by hydrochloric acid leaching-roasting process. Cold hydrochloric acid leaching did not completely remove impurities. After cold hydrochloric acid leaching, the specific surface area first increased slightly and then decreased significantly, while the specific surface area increased slightly after hot hydrochloric acid leaching. Moreover, compared with hot hydrochloric acid leaching, the decrease in specific surface area with the increase of roasting temperature below 1100°C was greater in cold hydrochloric acid leaching.

[0044] (4) Calcination-alkali leaching: The diatomite powder is purified by calcining first and then alkali leaching. It is calcined at 700-1200℃, mixed with a certain concentration of strong alkali (NaOH, KOH, LiOH) solution for reaction, and filtered and washed. The SiO content of the diatomite powder is significantly increased. Compared with acid leaching, this method does not introduce other impurities, is environmentally friendly, has less equipment corrosion, and has a simple process and low cost.

[0045] (5) Hot flotation-magnetic separation-acid cooking method: The second and third grade diatomite are purified through this process. The comprehensive application of the three methods removes mineral impurities and chemical impurities in the diatomite, improves the purity of the diatomite and improves the pore structure of the diatomite. Under the process conditions of strong scrubbing for 1 hour, sulfuric acid digestion for 3 hours, and sulfuric acid concentration of 15% to 20%, diatomite that meets the first grade soil standard was obtained.

[0046] (6) Scrubbing-microwave-acid leaching: Microwaves can accelerate the rate of chemical reactions. Adding microwaves to the acid leaching process can significantly improve the acid leaching effect. Microwaves were added to the acid leaching process of diatomite. Through systematic tests on conditions such as sulfuric acid concentration, microwave power, and leaching time, it was found that the main factor affecting leaching was the leaching time. The longer the leaching time, the higher the microwave power, and the greater the sulfuric acid concentration, the lower the Fe02 content in the diatomite. By first scrubbing, crushing, and dispersing the diatomite, then classifying and removing impurities, and finally acid leaching to remove iron under the action of microwaves, a filter aid product with qualified composition was obtained. The high efficiency of microwave acid leaching purification can reduce its action time by 10 times compared with conventional acid leaching purification. In addition, microwave pretreatment before acid leaching will also have better results than direct acid leaching without pretreatment.

[0047] like Figure 2 As shown, as a preferred embodiment, the S1 includes: S11, taking a certain amount of diatomaceous earth and soaking it for a certain period of time; S12, adding a certain concentration and a certain amount of sodium hydroxide as a dispersant to the soaked diatomite, so that the slurry concentration reaches 40%; S13, stirring and scrubbing the slurry to separate the debris minerals, clay minerals and diatoms, and precipitating sand-grade coarse soil, suspended clay and selected diatomaceous earth respectively, and by continuous scrubbing, the debris minerals and clay minerals are removed, the diatoms are relatively enriched, the silicon dioxide content is increased, and the aluminum oxide and iron oxide contents are reduced; S14, taking the diatomaceous earth that has been scrubbed 5-10 times and placing it in a centrifuge for centrifugation, discarding the supernatant after centrifugation, and collecting the purified diatomaceous earth precipitate.

[0048] In the present embodiment, specifically, 2000g of diatomite is first soaked for 5-6 hours, and then 3000g of 50% sodium hydroxide solution is used as a dispersant to make the slurry concentration up to 40%, and stirred and scrubbed to separate the debris minerals from the clay minerals and diatoms, and precipitate sand-grade coarse soil, suspended clay and selected diatomite respectively, and the scrubbing time is about 40-50 minutes each time, the time of sand-grade coarse soil is 6-8 minutes, and the time of diatomite is 6-7 hours. By scrubbing, the debris minerals and clay minerals are removed, diatoms are relatively enriched, the silicon dioxide content is increased, the aluminum oxide and iron oxide content are reduced, and the quality of diatomite is improved. The more times of scrubbing, the better the quality. The diatomite scrubbed for 5-10 times is placed in a centrifuge for centrifugation, and the parameters are set to 2000-3000rpm, 10-20min, and the supernatant is discarded after centrifugation to collect the purified diatomite precipitation.

[0049] S2, activating the purified diatomaceous earth, including: baking the purified diatomaceous earth at a first specific temperature range for a first specific time range for activation treatment; As a preferred embodiment, the first specific temperature range is 100-300°C.

[0050] As a preferred embodiment, the first specific time period ranges from 8 to 72 hours.

[0051] S3, alkalizing the activated diatomaceous earth, including: placing the activated and purified diatomaceous earth in an environment with a pH value of 7-11; S4, treating the alkalized diatomaceous earth with an anionic surfactant; like Figure 3 As shown, as a preferred embodiment, the S4 includes: S41, adding a treatment solution formed by the anionic surfactant to the alkalized diatomaceous earth; S42, after sufficient stirring, mixing, standing and centrifugation, the supernatant is discarded and the precipitate is collected.

[0052] As a preferred embodiment, the anionic surfactant includes but is not limited to one or more of the following substances: soap, alkylbenzene sulfonate, alkyl sulfonate ester salt, alkyl sulfonate, alkyl sulfate, fluorinated fatty acid salt, polysiloxane and fatty alcohol sulfate.

[0053] Working principle: Anionic surfactants form surface-active complexes or chelates with heavy metal ions in urine. Different anionic surfactants have selective complexation with different metal ions or the same anionic surfactant has selective complexation with different metal ions under different pH values ​​and other conditions, thereby flotation separation of inorganic salts and electrolytes in urine to remove interferences.

[0054] As a preferred embodiment, the standing time is 4-36 hours; the centrifugation is carried out by placing the mixture in a centrifuge, the centrifugation speed is 2000-3000 rpm, and the centrifugation time is 30-50 min.

[0055] S5, baking the diatomaceous earth treated with the anionic surfactant within a second specific temperature range and a second specific time range to perform activation treatment, and forming the solid adsorbent product after the activation treatment.

[0056] As a preferred embodiment, S5 includes: baking the precipitate collected in S42 in an electric constant temperature blast drying oven (in this embodiment, model 101-2-BS-Ⅱ; standard number Q / BKYY31-2000) at 100-300°C for 8-72 hours for activation treatment, and the prepared product is a solid adsorbent product. Embodiment 3

[0057] like Figure 4 As shown, this embodiment provides a urine purification device, comprising a carrying container, the carrying container comprising a tube body (3), the solid adsorbent for urine purification according to the first aspect of the present invention is filled inside the tube body (3); a liquid injection port (2) is arranged at the top of the tube body (3), and a plugging cap (1) for blocking the liquid injection port (2) is arranged above the liquid injection port (2); a liquid dripping port (4) is arranged below the liquid dripping port (4), and a lower cap (1) for blocking the liquid dripping port (4) is arranged below the liquid dripping port (4). The invention relates to a method for preparing a urine sample, wherein the urine sample is provided with a lower plug cap (5) at a tip of the dripping port (4); the diameter of the end of the dripping port (4) connected to the tube body (3) is larger than the diameter of the end of the dripping port (4) connected to the lower plug cap (5); a filter paper (10) is laid on the bottom of the tube body, the solid adsorbent is placed on the filter paper (10) and is in liquid communication with an inlet end with a larger diameter in the dripping port (4), so as to filter and purify urine flowing through the tube body to the dripping port (4), thereby reducing or eliminating errors caused by impurities in subsequent measurement of the iodine content in urine. Application Examples

[0058] 1. Preparation of urine purification device 1. Preparation of solid adsorbent Weigh 5.611g of potassium hydroxide (Sinopharm Chemical Reagent Co., Ltd. CAS: 1310-58-3) with an electronic balance and add it to 2000ml of deionized water, stirring slowly to fully dissolve. Weigh 200g of diatomaceous earth (Yuanye Biological, CAS: 91053-39-3, item number S30556, LOT: S05J8Y39285) with an electronic balance and add it to stir to fully dissolve. Centrifuge it in a centrifuge, set the parameters to 2000-3000rpm, 10-20min, discard the supernatant after centrifugation, and bake it in a 100-300℃ electric constant temperature blast drying oven (model; 101-2-BS-Ⅱ, standard number: Q / BKYY31-2000) for 8-72 hours for activation treatment. Take the activated diatomaceous earth at 5-10% g / V and add it to 20-30% g / V soap solution (commercially available, PH7-11. The soap base components are mainly divided into fatty acids and alkalis. Fatty acids include lauric acid, myristic acid, palmitic acid, (stearic acid), etc., and various oils of handmade soap, because they contain saturated and unsaturated fatty acids; the alkalis are mostly sodium hydroxide, potassium hydroxide, triethanolamine, etc.) and stir well and let stand for 4-36 hours. Place it in a centrifuge for centrifugation, set the parameters to 1000-2000rpm, 30-50min, discard the supernatant after centrifugation, and bake it in a 100-300℃ electric constant temperature blast drying oven (model; 101-2-BS-Ⅱ, standard number: Q / BKYY31-2000) for 8-72 hours for activation treatment.

[0059] Weigh 1-3g±0.2g of solid adsorbent with weighing paper on an electronic balance (BSA224S-CWMax220gd=0.1mg Sartorius Scientific Instruments (Beijing) Co., Ltd.) and add it to the interference removal device from the liquid injection port. Be careful not to spill it and cover the upper and lower plugs tightly.

[0060] Verification test Verification test 1: recovery rate comparison test

[0061] 1. Materials: 1. National standard substances (produced by the National Iodine Deficiency Disease Reference Laboratory GBW09108n, 76.9ug / L±7, GBW09109j, 155±15ug / L, GBW09110q, 232±23ug / L) 2. Urine iodine determination kit (peracetic acid tetramethylbenzidine oxidation colorimetric method) batch number 03230502, production date: 2023.05.23, expiration date: 2024.5.22 2. Methods: 1. Follow the instructions of the national standard material to prepare the standard curve.

[0062] 2. Sample preparation: 1) Preparation of mixed urine a) Control conditions: 20±2℃, healthy employees who have a normal diet and have not consumed excessive amounts of iodized salt and iodized food within 3 days, and preparation time limit within 8 hours.

[0063] b) Method: Collect urine from healthy employees of the company who have a normal diet and have not consumed excessive amounts of iodized salt and iodized food within 3 days, mix the urine, and filter it using purified filter paper → 0.45µm filter membrane in sequence within 8 hours. Measure the urine volume using a calibrated volumetric flask at 20±2℃, add a high-efficiency preservative to a value of 0.1% (V / V), and measure the urine iodine concentration (100ug / L±10). Store it in a sealed container under the same conditions and use it within 48 hours.

[0064] c) At 20±2℃ and relative humidity <40%, take a bottle of urine iodine national standard substance GBW09108n, accurately measure 5 ml of the mixed urine prepared by the above method, add it and dissolve and mix well.

[0065] d) At 20±2℃ and relative humidity <40%, take a bottle of urine iodine national standard substance GBW09109j and accurately measure 5 ml of the mixed urine prepared by the above method and add it to dissolve and mix.

[0066] e) At 20±2℃ and relative humidity <40%, take a bottle of urine iodine national standard substance GBW09110q, accurately measure 5 ml of the mixed urine prepared by the above method, add it and dissolve and mix well.

[0067] (III) Operation method: 1) Detect with a spectrophotometer at 660 nm and use water as blank to adjust to zero.

[0068] 2) Take 1.4ml of diluent (the components in the kit, measure 900mL of purified water to dissolve, add 12.8185g of citric acid, then add 4.4g of sodium hydroxide to dissolve, add 9g of sodium chloride to completely dissolve, and then add purified water to 1000ml.) and inject it into the interference removal device, then take 0.7ml of the dissolved national standard substance GBW09108n and inject it into the interference removal device. By shaking and mixing, the activated diatomaceous earth selectively adsorbs bilirubin, urea, hepatic anhydride, inorganic salts and electrolytes in urine, but does not adsorb iodine. Use a liquid pusher to push the interference-free diluted standard substance into the test tube.

[0069] Testing instrument: Mindray biochemical analyzer (BS-350S), testing kits: creatinine (Sino-Biotech Co., Ltd.); sodium (Jiuqiang Biotechnology Co., Ltd.); urea (Jiuqiang Biotechnology Co., Ltd.); urine microalbumin (Sino-Biotech Co., Ltd.); 3) Immediately add 150µl of color developing solution to the test tube, mix well, and add 30µl of complex oxidant.

[0070] 4) When the timing reaches 60 seconds accurately, read the absorbance as the absorbance of urine and calculate the concentration of urine iodine according to the formula.

[0071] 5) Take the dissolved national standards GBW09108n, 09109j, and 09110q and measure them three times each according to the above method.

[0072] Example: Y=aX+b (Y is urine iodine concentration, X is absorbance, a and b are constants, R 2 ≥0.95) Use the components in the kit according to the instructions to measure the absorbance and calculate the concentration of urinary iodine according to the formula.

[0073] The improved group is the urine iodine purification device of the present invention, and the control group is the urine iodine purification device made from (patent number: 2006100568250) Detection kits: All are from the kits produced by Beijing Zhongsheng Jinyu Company. Beijing Medical Device Registration No. 20172400527 Recovery rate: (measured urine iodine concentration - mixed urine iodine concentration / national standard concentration) * 100% 3. Experimental results: 1. Recovery rate test results (1) The specific values ​​of recovery rate are shown in Table 1: Table 1

[0074] (2) The paired sample verification results are shown in Table 2.

[0075] Table 2 Paired Sample Test (Recovery)

[0076] (3) SPSS22 paired sample t-test analysis The recovery rates of the control group and the improved group after purification were calculated, and it was found that the recovery rate of urine iodine after purification by the interference removal device (improved group) reached 95.4%, and the recovery rate of urine iodine after purification by the control group was 80.6%. The recovery rate of the kit manufactured by this technology increased by 14.82%, P < 0.01 and was statistically significant. This shows that the present invention can significantly improve the recovery rate in the process of urine iodine purification.

[0077] 2. Interference removal experiment and results (1) The comparison of the content before and after interference removal is shown in Table 3: Table 3

[0078] (2) Paired sample test data are shown in Table 4: Table 4

[0079] (3) SPSS22 paired sample t-test was used to analyze and calculate the concentration difference of each interference before and after purification, and the result was: This purification device can effectively reduce creatinine 13935umol / L, urea 18.9g / L, urine microalbumin 13.2; sodium 116.3mmol / LP <0.01 and is statistically significant.

[0080] This indicates that the present invention can remove the interference of creatinine, urea, urine microalbumin and sodium in urine.

[0081] The above method uses diatomaceous earth plus soap (anionic surfactant) soap solution (commercially available, PH7-11. The soap base components are mainly divided into fatty acids and alkalis. Fatty acids include lauric acid, myristic acid, palmitic acid, (stearic acid), etc., as well as various oils of handmade soaps, because they contain saturated and unsaturated fatty acids; the most common alkalis are sodium hydroxide, potassium hydroxide, triethanolamine, etc.) to adsorb and float to separate interferences in urine, so that the recovery rate of urine iodine reaches 95%.

[0082] Through the description of the above implementation methods, those skilled in the art can clearly understand that the above embodiments can be implemented by software, or by means of software plus necessary general hardware platforms. Based on such understanding, the technical solutions of the above embodiments can be embodied in the form of software products, which can be stored in a non-volatile storage medium (which can be a CD-ROM, a USB flash drive, a mobile hard disk, etc.), including several instructions for enabling a computer device (which can be a personal computer, a server, or a network device, etc.) to execute the methods described in the various embodiments of the present invention.

[0083] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A solid adsorbent for urine purification, characterized in that: include: Diatomaceous earth that has been subjected to purification, activation treatment, alkalization treatment, anionic surfactant treatment and baking activation treatment in sequence; wherein the activation treatment comprises baking the diatomaceous earth within a first specific temperature range for a first specific time range, the alkalization comprises placing the diatomaceous earth purified by the activation treatment in an environment with a pH value of 7-11, the anionic surface treatment comprises adding a treatment solution formed by the anionic surfactant to the diatomaceous earth that has been subjected to the alkalization treatment, and stirring, mixing, standing and centrifuging the treatment solution, discarding the supernatant and collecting the precipitate; the baking activation treatment comprises baking the diatomaceous earth treated with the anionic surfactant within a second specific temperature range for a second specific time range.

2. A method for preparing a solid adsorbent for urine purification according to claim 1, characterized in that: include: S1, purifying diatomite, comprising: adopting a single purification method or a combined purification method; the single purification method comprises: a scrubbing method, an acid leaching method, a roasting method, a magnetic separation method, a thermal sedimentation method or a thermal flotation method; the combined purification method comprises: a scrubbing-acid leaching method, a water washing-roasting method, a roasting-acid leaching method, a roasting-alkali leaching method, a thermal flotation-magnetic separation-acid boiling method and a scrubbing-microwave-acid leaching method; S2, activating the purified diatomaceous earth, including: baking the purified diatomaceous earth at a first specific temperature range for a first specific time range for activation treatment; S3, alkalizing the activated diatomaceous earth, including: placing the activated and purified diatomaceous earth in an environment with a pH value of 7-11; S4, treating the alkalized diatomaceous earth with an anionic surfactant; S5, baking the diatomaceous earth treated with the anionic surfactant within a second specific temperature range and a second specific time range to perform activation treatment, and forming the solid adsorbent product after the activation treatment.

3. The method for preparing a solid adsorbent for urine purification according to claim 2, characterized in that: The S1 includes: S11, taking a certain amount of diatomaceous earth and soaking it for a certain period of time; S12, adding a certain concentration and a certain amount of sodium hydroxide as a dispersant to the soaked diatomite, so that the slurry concentration reaches 40%; S13, stirring and scrubbing the slurry to separate the debris minerals, clay minerals and diatoms, and precipitating sand-grade coarse soil, suspended clay and selected diatomaceous earth respectively, and by continuous scrubbing, the debris minerals and clay minerals are removed, the diatoms are relatively enriched, the silicon dioxide content is increased, and the aluminum oxide and iron oxide contents are reduced; S14, taking the diatomaceous earth that has been scrubbed 5-10 times and placing it in a centrifuge for centrifugation, discarding the supernatant after centrifugation, and collecting the purified diatomaceous earth precipitate.

4. The method for preparing a solid adsorbent for urine purification according to claim 3, characterized in that: The first specific temperature range is 100-300°C.

5. The method for preparing a solid adsorbent for urine purification according to claim 4, characterized in that: The first specific time period ranges from 8 to 72 hours.

6. The method for preparing a solid adsorbent for urine purification according to claim 5, characterized in that: The S4 includes: S41, adding a treatment solution formed by the anionic surfactant to the alkalized diatomaceous earth; S42, after sufficient stirring, mixing, standing and centrifugation, the supernatant is discarded and the precipitate is collected.

7. The method for preparing a solid adsorbent for urine purification according to claim 6, characterized in that: The anionic surfactant includes, but is not limited to, one or more of the following: soap, alkylbenzene sulfonate, alkyl sulfonate ester salt, alkyl sulfonate, alkyl sulfate, fluorinated fatty acid salt, polysiloxane and fatty alcohol sulfate.

8. The method for preparing a solid adsorbent for urine purification according to claim 7, characterized in that: The standing time is 4-36 hours; the centrifugation is carried out by placing the mixture in a centrifuge, the centrifugal speed is 2000-3000 rpm, and the centrifugal time is 30-50 minutes.

9. The method for preparing a solid adsorbent for urine purification according to claim 8, characterized in that: The step S5 comprises: baking the precipitate collected in step S42 in an electric constant temperature forced air drying oven at 100-300° C. for 8-72 hours for activation treatment, and the solid adsorbent product is prepared.

10. A urine purification device is provided, comprising a carrying container, the carrying container comprising a tube body (3), the solid adsorbent for urine purification according to claim 1 being filled inside the tube body (3); a liquid injection port (2) is arranged at the top of the tube body (3), a plugging cap head (1) for blocking the liquid injection port (2) is arranged above the liquid injection port (2); a dripping port (4) is arranged below the tube body (3), a lower plugging cap (5) for blocking the lower tip of the dripping port (4) is arranged below the dripping port (4); the diameter of one end of the dripping port (4) connected to the tube body (3) is larger than the diameter of one end connected to the lower plugging cap (5); a filter paper (10) is laid at the bottom of the tube body, the solid adsorbent is placed on the filter paper (10) and is in liquid communication with an inlet end with a larger diameter in the dripping port (4), so as to filter and purify urine flowing to the dripping port (4) through the tube body.

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