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

Abstract

The application discloses a solid adsorbent for urine purification, which comprises diatomite which is sequentially subjected to purification, activation treatment, alkalization treatment, anion surfactant treatment and baking activation treatment; the activation treatment is baking for a first specific time duration range at a first specific temperature range; the alkalization treatment comprises placing the diatomite subjected to the activation treatment into an environment with a pH value of 7-11; the anion surfactant treatment is that anion surfactant is added into the diatomite subjected to the alkalization treatment to form a treatment liquid, and after sufficient stirring, mixing, standing and centrifugation, the supernatant is discarded and the precipitate is collected; and the baking activation treatment is baking for a second specific time duration range at a second specific temperature range. The application further discloses a preparation method of the solid adsorbent and a urine purification device, which comprises a bearing container, the bearing container comprises a tube body, the solid adsorbent for urine purification is filled in the tube body, a liquid injection port and a plug head are arranged at the top of the tube body, a liquid drop port and a lower plug head are arranged below, and filter paper is laid at the bottom of the tube body.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of removing interferents in urine, and particularly relates to a solid adsorbent for urine purification, a preparation method and a urine purification device. BACKGROUND

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

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

[0004] The components in urine are water, urea (molecular formula CH4N2O), uric acid (molecular formula C5H4N4O3), creatinine (molecular formula C4H7N3O), protein (a biological macromolecule 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 100-300 ug / L), other components in urine will interfere with the detection result, affect the recovery rate of urine iodine, and thus the content cannot be accurately detected. 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 inside. The selective specific adsorbent is an adsorbent composed of 0.2-1 g of purified activated carbon and 100-1000 ug of iodine adsorption antagonist, which is used for specific adsorption of interfering substances in urine. The purified activated carbon is soaked in a buffer solution, and the iodine adsorption antagonist is activated by baking at 70-250°C for 4-72 hours. However, this urine purification device can only adsorb part of the interfering substances in urine, and the recovery rate of urine iodine is low (i.e. some doses of iodine in urine are lost during the purification process), which still has a very great influence on the detection result, directly affecting the diagnosis and treatment of diseases, causing misdiagnosis and missed diagnosis. SUMMARY

[0005] The purpose of the present application is to overcome the defects of the prior art, aiming at the problems in the related art, provide a solid adsorbent for urine purification, preparation method and urine purification device, the solid adsorbent is treated by diatomite and alkali, and then roasted and activated by anion surfactant, the solid adsorbent is prepared by diatomite and anion surfactant (soap) after alkalization, and the activation treatment can remove most of the interfering substances in the urine, the urine purification device adopts the solid adsorbent, and the interfering substances (urea, uric acid, creatinine, glucose and protein) can be removed, the recovery test using national standard urine iodine material can reach 95%, the urine iodine detection result is accurate, and great help is provided for precise clinical diagnosis and treatment.

[0006] The first aspect of the present application is to provide a solid adsorbent for urine purification, comprising: diatomite sequentially subjected to purification, activation treatment, alkalization treatment, anion surfactant treatment and roasting and activation treatment; wherein the activation treatment is roasting for a first specific time range at a first specific temperature range, the alkalization comprises placing the purified diatomite subjected to the activation treatment in an environment with a pH value of 7-11, the anion surface treatment is a treatment liquid formed by adding the anion surfactant to the diatomite subjected to the alkalization treatment, and after sufficient stirring, mixing, standing and centrifugation, the supernatant is discarded and the precipitate is collected; and the roasting and activation treatment is roasting for a second specific time range at a second specific temperature range.

[0007] The second aspect of the present application is to provide a preparation method of a solid adsorbent for urine purification, comprising:

[0008] S1, purifying diatomite, comprising: using a single purification method or a combined purification method; the single purification method comprises scrubbing, acid leaching, calcination, magnetic separation, thermal sedimentation or thermal flotation; and the combined purification method comprises scrubbing-acid leaching, water washing-calcination, calcination-acid leaching, calcination-alkali leaching, thermal flotation-magnetic separation-acid boiling and scrubbing-microwave-acid leaching;

[0009] S2, activating the purified diatomite, comprising: roasting the purified diatomite at a first specific temperature range for a first specific time range to activate the diatomite;

[0010] S3, alkalizing the diatomite subjected to the activation treatment, comprising: placing the purified diatomite subjected to the activation treatment in an environment with a pH value of 7-11;

[0011] S4, treating the diatomite subjected to the alkalization treatment by an anion surfactant;

[0012] S5, baking the diatomite treated with the anionic surfactant in a second specific temperature range for a second specific time range to perform an activation treatment, and forming the solid adsorbent finished product after the activation treatment.

[0013] Preferably, the S1 comprises:

[0014] S11, soaking a certain amount of diatomite for a certain time;

[0015] S12, adding a certain concentration and amount of sodium hydroxide as a dispersant to the soaked diatomite, so that the slurry concentration reaches 40%;

[0016] S13, stirring and scrubbing the slurry to separate the detrital minerals and clay minerals from the diatom, and respectively precipitating the sand grade coarse soil, the suspended grade clay, and the selected diatomite. Through continuous scrubbing, the detrital minerals and clay minerals are removed, the diatom is relatively enriched, the content of silicon dioxide is increased, and the content of aluminum oxide and iron oxide is reduced.

[0017] S14, placing the diatomite scrubbed for 5-10 times in a centrifuge for centrifugation, and collecting the purified diatomite precipitate after discarding the supernatant.

[0018] Preferably, the first specific temperature range is 100-300°C.

[0019] Preferably, the first specific time range is 8-72 hours.

[0020] Preferably, the S4 comprises:

[0021] S41, adding the treatment solution formed by the anionic surfactant to the diatomite treated by the alkalization treatment;

[0022] S42, after sufficient stirring, mixing, standing, and centrifugation, discarding the supernatant and collecting the precipitate.

[0023] Preferably, the anionic surfactant includes but is not limited to one or more of the following: soap, alkyl benzene sulfonate, alkyl sulfonate, alkyl sulfonate, alkyl sulfate, fluorine-containing fatty acid salt, polysiloxane, and fatty alcohol sulfate.

[0024] Preferably, the standing time is 4-36 hours; the centrifugation is performed by placing in a centrifuge, the speed of the centrifugation is 2000-3000 rpm, and the time of the centrifugation is 30-50 min.

[0025] Preferably, the S5 comprises: baking the precipitate collected in S42 in a 100-300°C electric heating constant temperature drying oven for 8-72 hours to perform an activation treatment, and the prepared product is the solid adsorbent finished product.

[0026] The third aspect of the present application provides a urine purification device, comprising a carrying container, the carrying container comprises a tube body (3), the solid adsorbent for urine purification according to the first aspect of the present application is filled in the inside of the tube body (3); the top of the tube body (3) is provided with a liquid injection port (2), the upper side of the liquid injection port (2) is provided with a plug cap (1) for plugging the liquid injection port (2); the lower side of the tube body (3) is provided with a liquid drop port (4), the lower side of the liquid drop port (4) is provided with a lower plug cap (5) for plugging the lower end of the liquid drop port (4); the diameter of the end of the liquid drop port (4) connected with the tube body (3) is greater than the diameter of the end connected with the lower plug cap (5); the bottom of the tube body is paved with filter paper (10), the solid adsorbent is placed on the filter paper (10) and is in liquid communication with the inlet end of the liquid drop port (4) with a larger diameter, for filtering and purifying the urine flowing to the liquid drop port (4) through the tube body.

[0027] The solid adsorbent, the preparation method and the urine purification device of the present application have the following beneficial effects:

[0028] The interference in the urine is removed by alkali treatment of diatomite and activation of an anionic surfactant, the solid adsorbent is treated by alkali treatment of diatomite and activation of an anionic surfactant (soap), most of the interference in the urine can be removed by alkali treatment of diatomite and activation of an anionic surfactant (soap), and the urine purification device uses the solid adsorbent, which can remove the interference (urea, uric acid, creatinine, glucose and protein), the recovery test using the national standard material of urinary iodine can reach 95%, the detection result of urinary iodine is accurate, and great help is provided for precise clinical diagnosis and treatment. BRIEF DESCRIPTION OF DRAWINGS

[0029] In order to more clearly illustrate the technical solutions in the specific embodiments or related art, the following will briefly introduce the drawings needed to be used in the specific embodiments or related art description. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0030] Figure 1 The preparation method flowchart of the solid adsorbent for urine purification provided according to the embodiment of the present application is shown.

[0031] Figure 2 The preparation method flowchart of the solid adsorbent for urine purification provided according to the embodiment of the present application is shown.

[0032] Figure 3A flowchart of step S4 in the preparation method of the solid adsorbent for urine purification provided according to the embodiment of the present application.

[0033] Figure 4 A structural diagram of the urine purification device provided according to the embodiment of the present application. DETAILED DESCRIPTION

[0034] The technical solutions of the present application will be described clearly and completely below with reference to the drawings. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative efforts fall within the scope of protection of the present application.

[0035] In the description of the present application, it should be noted that the orientations or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and therefore cannot be understood as indicating or implying that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation on the present application. In addition, the terms "first", "second", "third" are only for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0036] In the description of the present application, it should be noted that unless otherwise explicitly specified and limited, the terms "mounting", "connecting", "connection" should be understood broadly, for example, it can be fixed connection, or detachable connection, or integrally connected; it can be mechanical connection, or electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, or the internal communication of two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0037] The term "about" is used herein in connection with a value to include normal variation in measurement by a person skilled in the art, and should be understood to have the same meaning as "approximately" and cover a typical error range, for example, ±5% of the specified value.

[0038] The terms such as "one", "a", and "the" are not intended to refer only to a single entity, but include a general category that can be illustrated using a specific example.

[0039] Unless otherwise specified, any amount (e.g., concentration) of a component in a composition given in percentage (%) refers to weight percentage per volume. Example One

[0040] The embodiment provides a solid adsorbent for urine purification, comprising: diatomite sequentially subjected to purification, activation treatment, alkalization treatment, anion surfactant treatment and baking activation treatment; wherein the activation treatment is baking for a first specific time length range at a first specific temperature range, the alkalization comprises placing the diatomite subjected to the activation treatment in an environment with a pH value of 7-11, the anion surface treatment is that after the treatment liquid formed by adding the anion surfactant into the diatomite subjected to the alkalization treatment is fully stirred, uniformly mixed, placed and centrifuged, the supernatant is discarded and the precipitate is collected; and the baking activation treatment is that the diatomite subjected to the anion surfactant treatment is baked for a second specific time length range at a second specific temperature range.

[0041] Working principle of the solid adsorbent for urine purification:

[0042] (1) Removal of interfering substances (urea, uric acid, creatinine, glucose, protein) in urine:

[0043] (1) Urea: Urea is easily soluble in water and can be hydrolyzed into ammonia and carbon dioxide under the action of acid, alkali and enzyme (acid and alkali need to be heated). The sodium hydroxide on the diatomite reacts with it when the urine is added to the interference removal device, so as not to affect the detection of iodine in urine. The chemical formula of urea is CO(NH2)2.

[0044] CO(NH2)2+NaOH→Na2CO3+2NH3+H2O;

[0045] (2) Uric acid: Uric acid is the main metabolic product of birds and reptiles and is slightly soluble in water and easy to form crystals. The main product in normal human urine is urea, containing a small amount of uric acid. Under the action of sodium hydroxide in diatomite, the detection of iodine in urine will not be affected. The chemical formula of uric acid is C5H4N4O3.

[0046] C5H4N4O3+NaOH→Na2CO3+2NH3+H2O;

[0047] (3) Creatinine: Creatinine is a compound produced in the process of muscle energy production and is metabolized from phosphocreatine. Normal kidney function can filter and excrete creatinine in the blood. Therefore, the level of creatinine in the blood reflects the filtration function of the kidney and is an indicator for detecting kidney function. Creatinine level is affected by many factors, including age, race, gender and body type. Blood creatinine may increase or decrease under different diseases and physiological conditions. The chemical formula of creatinine is C4H7N3O.

[0048] C5H4N4O3+NaOH→Na2CO3+2NH3+H2O;

[0049] (4) Glucose: It is the most widely distributed monosaccharide in nature. Glucose contains five hydroxyl groups and an aldehyde group, with the properties of polyols and aldehydes. It is easily decomposed under alkaline conditions; urine is added to the urine purification device, and the sodium hydroxide in diatomite is alkaline, which causes it to decompose without affecting the detection of iodine in urine, and the chemical formula of glucose is C6H 12 O6.

[0050] C6H 12 O6+NaOH→C6H 11 O6Na+H2O

[0051] (5) Protein: Urinary proteins include immunoglobulins, albumin, and retinol-binding proteins. Urine is added to the interference removal device, and the sodium hydroxide and silicon hydroxyl groups on diatomite 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 being filtered out, so it does not affect the detection of iodine in urine, and the chemical formula of protein is Pr.

[0052] Pr+NaOH→precipitate→water

[0053] (6) Iodine: Iodine is less active than its homologous elements F2, Cl2, and Br2, and has the smallest solubility in water, only slightly soluble in water, with a solubility of 0.029 g / 100 g of water. I2 can undergo self-oxidation and reduction under alkaline conditions to generate iodate IO3 - and iodine ions I - :

[0054] 3I2+6OH - →5I - +IO3 - +3H2O

[0055] This is because there is no hypoiodite IO - in the solution. At any temperature, IO - rapidly undergoes self-oxidation and reduction to generate I - and IO3 - . Therefore, the iodine in urine can be detected without being affected.

[0056] (II) Diatomite also has strong adsorption capacity, low thermal conductivity, and good chemical stability. Example Two

[0057] As shown in the description, the present embodiment provides a preparation method of a solid adsorbent for urine purification, comprising: Figure 1

[0058] S1, purifying diatomite, comprising: using a single purification method or a combined purification method.

[0059] ​Diatom is a kind of single-cell algae, its individual is very small, generally 1m to several mm. When this aquatic plant dies, its debris is deposited in the ocean or lake, forming diatomite. The main component of diatomite is SiO, in the form of SiO·nH2O, also contains a small amount of Al, Fe, Ca, Mg, Na, K, P, etc., and individual metal impurities such as Cr, Ba, etc.

[0060] The single purification method comprises:

[0061] (1) Scrubbing method: proper scrubbing can finely grind and disperse the raw material particles without damaging the diatom shell. Mineral impurities such as clay that are solidified on the diatom shell are separated under the action of scrubbing, and after classification, the mineral impurities such as clay are removed, so that the content of SiO2 is increased. The more the scrubbing times, the better the cleaning effect, and the higher the SiO2 content of the diatomite obtained.

[0062] (2) Acid leaching method: acid leaching generally uses a mixed acid of hydrofluoric acid and sulfuric acid. Strong acid dissolves A12O3, Fe2O3, CaO, MgO and other impurities in diatomite to form salts. It is found that when hydrochloric acid is used for acid leaching of Turkish diatomite, with the increase of acid concentration and acid leaching time, A12O3, Fe2O3, CaO, MgO and other impurities are dissolved in hydrochloric acid, while a certain amount of amorphous SiO2 is also dissolved, and the dissolution of SiO2 is 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, but the amount of acid and water used in the treatment of diatomite is large, and the cost is relatively high.

[0063] (3) Roasting method: the roasting method is mainly used for beneficiation and purification of high loss on ignition type diatomite. When the roasting temperature is 600-800℃, the content of SiO2 can be significantly improved due to the volatilization of organic matter, and the pore size and surface acid strength are increased. The specific surface area reaches the maximum when the roasting temperature is 450℃, and the diatom shell will be damaged when the roasting temperature is higher than 900℃.

[0064] In addition, there are magnetic separation method, thermal sedimentation method, thermal flotation method, etc., and the combined purification method is preferably adopted.

[0065] The combined purification method comprises:

[0066] (1) Scrubbing-acid leaching: For low-grade diatomite, scrubbing and acid leaching are used for purification. 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%.

[0067] (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. Quartz, feldspar and clay impurities are removed by water washing, and organic matter is removed by roasting at 600℃. The number of water washings, water washing temperature, dispersant dosage and roasting temperature are tested. Finally, the SiO2 content in the diatomite is increased from 64.22% to 82.98%.

[0068] (3) Calcination-acid leaching: A roasting-acid leaching purification test was conducted on diatomite from a company in Jilin Province. A diatomite with a SiO content of over 90% was obtained. The study found that below 450°C, the specific surface area of ​​diatomite increased with increasing roasting temperature. After exceeding 450°C, the specific surface area decreased with increasing roasting temperature. The optimum concentration of sulfuric acid was 72%. Through testing and analysis, it was found that after purification, most of the impurities in the original diatomite were removed, the porosity improved, the specific surface area increased, and the adsorption performance increased. Turkish diatomite was purified using a hydrochloric acid leaching-calcination 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 after hot hydrochloric acid leaching, the specific surface area increased slightly. Moreover, compared with hot hydrochloric acid leaching, the specific surface area decreased more significantly below 1100°C with increasing roasting temperature.

[0069] (4) Calcination-alkaline leaching: The diatomite powder is purified by calcining first and then alkali leaching. The powder is calcined at 700-1200°C, then 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 low equipment corrosion, and is simple in process and low in cost.

[0070] (5) Hot flotation-magnetic separation-acid digestion method: This process is used to purify the second and third grade diatomite. The combined application of these three methods removes mineral and chemical impurities from the diatomite, improving the purity of the diatomite and 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.

[0071] (6) Scrubbing-microwave-acid leaching: Microwave can accelerate the chemical reaction rate, and the acid leaching effect can be significantly improved by adding microwave action during the acid leaching process. In the process of acid leaching of diatomite, by systematically testing the conditions such as sulfuric acid concentration, microwave power and leaching time, it is found that the main factor affecting leaching is leaching time, the longer the leaching time, the higher the microwave power and the greater the sulfuric acid concentration, the lower the Fe0 content in diatomite. Through the process of scrubbing, dispersing and dispersing diatomite first, then removing impurities by classification, and finally removing iron by acid leaching under the action of microwave, the qualified filter aid product is obtained in composition. The high efficiency of microwave acid leaching makes the action time 10 times less than that of conventional acid leaching. In addition, the effect of microwave pretreatment before acid leaching is better than that of direct acid leaching without pretreatment.

[0072] As shown in Figure 2 as a preferred embodiment, S1 comprises:

[0073] S11, a certain amount of diatomite is soaked for a certain time;

[0074] S12, a certain concentration and amount of sodium hydroxide is added to the soaked diatomite as a dispersant, so that the slurry concentration reaches 40%;

[0075] S13, the slurry is stirred and scrubbed to separate the detrital minerals and clay minerals from the diatom, and the sand grade coarse soil, suspended grade clay and selected diatomite are precipitated, respectively. Through continuous scrubbing, the detrital minerals and clay minerals are removed, the diatom is relatively enriched, the content of silicon dioxide is increased, and the contents of aluminum oxide and iron oxide are reduced;

[0076] S14, the diatomite scrubbed for 5-10 times is placed in a centrifuge for centrifugation, and the supernatant is discarded after centrifugation to collect the purified diatomite precipitate.

[0077] In this embodiment, 2000g of diatomite is first soaked for 5-6 hours, then 3000g of 50% sodium hydroxide solution is used as a dispersant to make the slurry concentration reach 40%, and the slurry is stirred and scrubbed to separate the detrital minerals and clay minerals from the diatom, and the sand grade coarse soil, suspended grade clay and selected diatomite are precipitated, respectively. The scrubbing time is about 40-50 minutes each time, the sand grade coarse soil time is 6-8 minutes, and the diatomite time is 6-7 hours. Through scrubbing, the detrital minerals and clay minerals are removed, the diatom is relatively enriched, the content of silicon dioxide is increased, and the contents of aluminum oxide and iron oxide are reduced, and the quality of diatomite is improved. The more the number 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 2000-3000 rpm and 10-20 min. After centrifugation, the supernatant is discarded to collect the purified diatomite precipitate.

[0078] S2, activating the purified diatomite, comprising: baking the purified diatomite at a first specific temperature range for a first specific time range;

[0079] As a preferred embodiment, the first specific temperature range is 100-300℃.

[0080] As a preferred embodiment, the first specific time range is 8-72 hours.

[0081] S3, alkali treatment of the activated diatomite, comprising: placing the purified diatomite after the activation treatment in an environment with a pH value of 7-11;

[0082] S4, treating the diatomite after the alkali treatment with an anionic surfactant;

[0083] As shown in Figure 3 As a preferred embodiment, S4 comprises:

[0084] S41, adding the anionic surfactant to the diatomite after the alkali treatment to form a treatment solution;

[0085] S42, after sufficient stirring, mixing, standing and centrifugation, discarding the supernatant and collecting the precipitate.

[0086] As a preferred embodiment, the anionic surfactant includes but is not limited to one or more of the following: soap, alkyl benzene sulfonate, alkyl sulfonate, alkyl sulfonate, alkyl sulfate, fluorine-containing fatty acid salt, polysiloxane and fatty alcohol sulfate.

[0087] Working principle: the anionic surfactant forms a complex or chelate with heavy metal ions in urine, and different anionic surfactants have selective complexing properties for different metal ions or the same anionic surfactant has selective complexing properties for different metal ions under different pH conditions, etc., so as to remove interference substances by flotation separation of inorganic salts and electrolytes in urine.

[0088] As a preferred embodiment, the standing time is 4-36 hours; the centrifugation is processed by placing it in a centrifuge, the speed of the centrifugation is 2000-3000 rpm, and the time of the centrifugation is 30-50 min.

[0089] S5, baking the diatomite after the anionic surfactant treatment at a second specific temperature range for a second specific time range to activate the diatomite, and forming the solid adsorbent finished product after the activation treatment.

[0090] As a preferred embodiment, the S5 comprises: baking the precipitate collected in S42 in a 100-300℃ electric heating constant temperature blast drying oven (in this embodiment, the model is 101-2-BS-II; the standard is Q / BKYY31-2000) for 8-72 hours for activation treatment, and the prepared is the solid adsorbent finished product. Example Three

[0091] As shown in Figure 4 the embodiment, the urine purification device comprises a bearing container, the bearing container comprises a tube body (3), the solid adsorbent for urine purification according to the first aspect of the application is filled in the tube body (3); a liquid injection port (2) is arranged at the top of the tube body (3), a cap head (1) for plugging the liquid injection port (2) is arranged above the liquid injection port (2); a liquid drop port (4) is arranged below the tube body (3), a lower plug cap (5) for plugging the lower tip of the liquid drop port (4) is arranged below the liquid drop port (4); the diameter of the end of the liquid drop port (4) connected with the tube body (3) is greater than the diameter of the end connected with the lower plug cap (5); 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 the entrance end of the liquid drop port (4) with a larger diameter, for filtering and purifying the urine flowing to the liquid drop port (4) through the tube body, so as to reduce or eliminate the error caused by impurities in the subsequent measurement of the iodine element content in the urine.

[0092] Application Example

[0093] I. Preparation of the urine purification device

[0094] (I) Preparation of the solid adsorbent

[0095] Weigh 5.611 g of potassium hydroxide (National Pharmaceutical Group Chemical Reagents Co., Ltd. CAS: 1310-58-3) into 2000 ml of deionized water, slowly stir to dissolve completely. Weigh 200 g of diatomite (Source Leaf Biology, CAS: 91053-39-3, item number S30556, LOT: S05J8Y39285) into the stirring solution and dissolve completely. Centrifuge in a centrifuge with parameters set at 2000-3000 rpm for 10-20 min, discard the supernatant after centrifugation, and bake in a 100-300°C electric heating constant temperature air drying oven (model: 101-2-BS-II, standard number: Q / BKYY31-2000) for 8-72 hours for activation treatment. Take the activated diatomite and add it to 20-30% g / V soap solution (marketed, PH 7-11. The soap base components mainly include fatty acids and alkali agents, fatty acids include lauric acid, myristic acid, palmitic acid, (stearic acid), etc., and various oils for handmade soap, containing saturated and unsaturated fatty acids; the most common alkali agents are sodium hydroxide, potassium hydroxide, triethanolamine, etc.). Mix well and let stand for 4-36 hours. Centrifuge in a centrifuge with parameters set at 1000-2000 rpm for 30-50 min, discard the supernatant after centrifugation, and bake in a 100-300°C electric heating constant temperature air drying oven (model: 101-2-BS-II, standard number: Q / BKYY31-2000) for 8-72 hours for activation treatment.

[0096] Weigh 1-3 g ± 0.2 g of solid adsorbent on an electronic balance (BSA224S-CW Max220gd = 0.1 mg Sartorius Scientific Instruments (Beijing) Co., Ltd.) using weighing paper, and add it to the interference-free device from the liquid injection port, taking care not to spill it. Tighten the upper and lower plug caps.

[0097] Verification test

[0098] Verification test 1: recovery rate comparison test

[0099] (I) Materials:

[0100] 1. National standard materials (GBW09108n, 76.9 ug / L ± 7, GBW09109j, 155 ± 15 ug / L, GBW09110q, 232 ± 23 ug / L produced by the National Iodine Deficiency Disease Reference Laboratory)

[0101] 2. Urine iodine determination kit (tetramethylbenzidine peroxoacetic acid oxidation colorimetric method) batch number 03230502, production date: 2023.05.23, expiration date: 2024.5.22

[0102] (II) Methods:

[0103] 1. According to the national standard material instruction book, make a standard curve.

[0104] 2. Sample preparation:

[0105] 1) Mixed urine preparation

[0106] a) Control conditions: 20±2℃, healthy employees with normal diet for 3 days, no excessive intake of iodine-containing salt and iodine-containing food, within 8 hours of preparation work.

[0107] b) Method: Collect the urine of healthy employees of the company who have normal diet for 3 days, no excessive intake of iodine-containing salt and iodine-containing food, mix, and within 8 hours, use purified filter paper→0.45µm filter membrane to filter, use calibrated volumetric flask to measure the volume of urine under the condition of 20±2℃, add high-efficiency preservative to 0.1% (V / V), measure the urine iodine concentration (100ug / L±10), seal under the same conditions, and use within 48 hours.

[0108] c) Under the condition of 20±2℃ and relative humidity <40%, take 5ml of mixed urine prepared by the above method and add it to a bottle of national standard material GBW09108n, dissolve and mix well.

[0109] d) Under the condition of 20±2℃ and relative humidity <40%, take 5ml of mixed urine prepared by the above method and add it to a bottle of national standard material GBW09109j, dissolve and mix well.

[0110] e) Under the condition of 20±2℃ and relative humidity <40%, take 5ml of mixed urine prepared by the above method and add it to a bottle of national standard material GBW09110q, dissolve and mix well.

[0111] (Three) Operation method:

[0112] 1) Use a 660nm spectrophotometer to detect, use water as a blank to zero.

[0113] 2) Take 1.4ml of diluent (a component in the kit, take 900mL purified water, dissolve and add citric acid 12.8185g, then add sodium hydroxide 4.4g, dissolve, add sodium chloride 9g, completely dissolve, and add purified water to 1000ml.) and inject into the interference removal device, then take 0.7ml of dissolved national standard material GBW09108n and inject into the interference removal device, mix by shaking, and selectively adsorb bilirubin, urea, liver dialysate, inorganic salt and electrolyte in the urine through activated diatomite, and do not adsorb iodine. Use a liquid pusher to push the interference-removed dilution standard material into the test tube.

[0114] Detection instrument: Mindray biochemical instrument (BS-350S), detection reagent kit: creatinine (Zhongsheng North Control Biotechnology Co., Ltd.); Sodium (Jiujiang Biotechnology Co., Ltd.); Urea (Jiujiang Biotechnology Co., Ltd.); Urinary microalbumin (Zhongsheng North Control Biotechnology Co., Ltd.);

[0115] 3) Immediately add 150ul of chromogenic solution to the test tube, mix well, and add 30ul of composite oxidant.

[0116] 4) When the accurate timing reaches 60 seconds, read the absorbance as the urine absorbance, and calculate the concentration of urinary iodine according to the formula.

[0117] 5) Respectively take the dissolved national standard GBW09108n, 09109j, 09110q according to the above method, and measure three times.

[0118] Example: Y=aX+b (Y is the concentration of urinary iodine, X is the absorbance, a and b are constants, R 2 ≥0.95)

[0119] The absorbance is measured by using the components in the kit according to the instructions, and the concentration of urinary iodine is calculated according to the formula.

[0120] The improved group is the urinary iodine purification device of the present application, and the control group is the urinary iodine purification device from (patent number: 2006100568250)

[0121] Detection reagent kit: all from Beijing Zhongsheng Kingue Company's reagent kit Beijing Shengjin Quan 20172400527

[0122] Recovery rate: (measured urinary iodine concentration-mixed urine urinary iodine concentration / national standard concentration)*100%

[0123] Three, experimental results:

[0124] 1, the recovery rate of experimental results

[0125] (1) The specific numerical value of the recovery rate is shown in Table 1:

[0126] Table 1

[0127]

[0128] (2) The paired sample verification results are shown in Table 2.

[0129] Table 2

[0130] Paired sample test (recovery rate)

[0131]

[0132] (3) Paired sample t test analysis by SPSS22

[0133] The recovery rates of the control group and the improved group after purification are calculated, and it is found that the recovery rate of urine iodine after purification of the interference removal device (the improved group) is 95.4%, the recovery rate of urine iodine after purification of the control group is 80.6%, the recovery rate of the kit manufactured by the present application is increased by 14.82%, P<0.01 and has statistical significance. It is proved that the present application can significantly improve the recovery rate in the purification process of urine iodine.

[0134] 2. Interference removal experiment and results

[0135] (1) The content comparison before and after interference removal is shown in Table 3:

[0136] Table 3

[0137]

[0138] (2) The paired sample test data are shown in Table 4:

[0139] Table 4

[0140]

[0141] (3) The concentration difference of each interference before and after purification is calculated by using SPSS22 paired sample t test analysis, and it is found that the present purification device can effectively reduce creatinine 13935 umol / L, urea 18.9 g / L, urine trace albumin 13.2, and sodium 116.3 mmol / L in urine, P<0.01 and has statistical significance.

[0142] It is proved that the present application can remove the interference of creatinine, urea, urine trace albumin and sodium in urine.

[0143] The above uses diatomite plus soap (anionic surfactant) soap solution (commercially available, PH 7-11. The soap base components are mainly divided into fatty acid and alkali, the fatty acid includes lauric acid, myristic acid, palmitic acid, (stearic acid) and various oils of handmade soap, because it contains saturated and unsaturated fatty acids; the alkali components are mainly sodium hydroxide, potassium hydroxide, triethanolamine, etc.). The interference in urine is adsorbed and separated by flotation, so that the recovery rate of urine iodine reaches 95%.

[0144] Those skilled in the art can clearly understand the above-mentioned embodiments can be realized by software, also can be realized by means of software plus necessary general hardware platform through the description of the above embodiments. Based on such understanding, the technical solutions of the above-mentioned embodiments can be embodied in the form of software product, which can be stored in a non-volatile storage medium (which can be CD-ROM, U disk, mobile hard disk, etc.), including a plurality of instructions to make a computer device (which can be a personal computer, server, or network device, etc.) execute the method described in each embodiment of the present application.

[0145] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, rather than limit them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement for part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for preparing a solid adsorbent for urine purification, characterized in that the solid adsorbent for urine purification comprises diatomite sequentially subjected to purification, activation treatment, alkalization treatment, anion surfactant treatment and baking activation treatment; wherein the activation treatment is baking for a first specific time range at a first specific temperature range, the alkalization treatment comprises placing the diatomite purified by the activation treatment in an environment with a pH value of 7-11, the anion surfactant treatment is adding a treatment solution formed by the anion surfactant to the diatomite subjected to the alkalization treatment, and then performing sufficient stirring, mixing, standing and centrifugation, discarding the supernatant and collecting the precipitate; and the baking activation treatment is baking for a second specific time range at a second specific temperature range for the diatomite subjected to the anion surfactant treatment. The method comprises: S1, purifying diatomite, comprising: using a single purification method or a combined purification method; the single purification method comprises scrubbing, acid leaching, calcination, magnetic separation, thermal sedimentation or thermal flotation; and the combined purification method comprises scrubbing-acid leaching, water washing-calcination, calcination-acid leaching, calcination-alkali leaching, thermal flotation-magnetic separation-acid boiling and scrubbing-microwave-acid leaching; S2, activating the purified diatomite, comprising: baking the purified diatomite at a first specific temperature range for a first specific time range to perform activation treatment; S3, alkalizing the diatomite subjected to the activation treatment, comprising: placing the diatomite purified by the activation treatment in an environment with a pH value of 7-11; S4, treating the diatomite subjected to the alkalization treatment with an anion surfactant; S5, baking the diatomite subjected to the anion surfactant treatment at a second specific temperature range for a second specific time range to perform activation treatment, and forming the solid adsorbent product after the activation treatment; The S1 comprises: S11, soaking a certain amount of diatomite for a certain time; S12, adding a certain concentration and 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 detrital minerals and clay minerals from the diatomite, and respectively precipitate the sand-grade coarse soil, the suspended-grade clay and the selected diatomite, through continuous scrubbing, the detrital minerals and clay minerals are removed, the diatomite is relatively enriched, the content of silicon dioxide is increased, and the contents of aluminum oxide and iron oxide are reduced; S14, placing the diatomite subjected to 5-10 times of scrubbing in a centrifuge for centrifugation, and collecting the purified diatomite precipitate after discarding the supernatant; The S4 comprises: S41, adding a treatment solution formed by the anion surfactant to the diatomite subjected to the alkalization treatment; S42, performing sufficient stirring, mixing, standing and centrifugation, discarding the supernatant and collecting the precipitate; The S5 comprises: baking the precipitate collected in S42 in a 100-300℃ electric constant-temperature air drying oven for 8-72 hours to perform activation treatment, and the prepared product is the solid adsorbent product. ​ The first specific temperature range is 100-300℃; the first specific time range is 8-72 hours.

2. The method for preparing a solid adsorbent for urine purification according to claim 1, characterized by, The anionic surfactant includes one or more of the following: soap, alkyl benzene sulfonate, alkyl sulfonate, alkyl sulfonate, alkyl sulfate, fluorine-containing fatty acid salt, polysiloxane and fatty alcohol sulfate.

3. The method for the preparation of solid adsorbents for urine purification according to claim 2, characterized in that, The standing time is 4-36 hours; the centrifugation is treated by placing in a centrifuge, the speed of the centrifugation is 2000-3000 rpm, and the time of the centrifugation is 30-50 min.

4. A urine purification device, characterized by, The solid adsorbent for urine purification of claim 1 is used for urine purification, comprising: a carrying container, the carrying container comprises a tube body (3), the solid adsorbent for urine purification is filled in the tube body (3); a liquid injection port (2) is arranged at the top of the tube body (3), a plug cap (1) for plugging the liquid injection port (2) is arranged above the liquid injection port (2); a liquid drop port (4) is arranged below the tube body (3), and a lower plug cap (5) for plugging the lower tip of the liquid drop port (4) is arranged below the liquid drop port (4); the diameter of one end of the liquid drop port (4) connected with the tube body (3) is greater than the diameter of the other end connected with the lower plug 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 the larger-diameter inlet end of the liquid drop port (4), for filtering and purifying the urine flowing to the liquid drop port (4) through the tube body; wherein the solid adsorbent for urine purification comprises diatomite which is sequentially subjected to purification, activation treatment, alkalization treatment, anionic surfactant treatment and baking activation treatment; the activation treatment is baked in a first specific temperature range for a first specific time range, the alkalization comprises placing the diatomite purified by the activation treatment in an environment with a pH value of 7-11, the anionic surfactant treatment comprises adding a treatment liquid formed by the anionic surfactant to the diatomite subjected to the alkalization treatment, and then fully stirring, uniformly mixing, standing and centrifuging, discarding the supernatant and collecting the precipitate; the baking activation treatment is baking the diatomite subjected to the anionic surfactant treatment in a second specific temperature range for a second specific time range.

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