An analysis method for the self-hydrolysis degree of titanium liquid

Abstract

The present invention provides a method for analyzing the self-hydrolysis degree of titanium solution. The analysis method includes: adding distilled water to the titanium solution, recording the time when the solution becomes turbid after the hydrolysis of the titanium solution, then obtaining the weight of the residue through filtration, calcination, and weighing, and finally calculating a numerical value using a formula, and using this numerical value to represent the degree of turbidity of the titanium solution, so as to determine the self-hydrolysis degree of the titanium solution. The method provided by the present invention can measure the self-hydrolysis degree of the titanium solution, which is fast, simple and effective, suitable for rapid analysis in the production line, and makes up for the deficiency of the quality analysis of the titanium solution.

Description

Technical Field

[0001] The present invention belongs to the technical field of titanium liquid quality analysis, and particularly relates to a method for analyzing the self-hydrolysis degree of titanium liquid. Background Art

[0002] In the production of titanium dioxide by the sulfuric acid method, sulfuric acid reacts with titanium ore to produce a black titanium oxysulfate solution (hereinafter referred to as titanium liquid). After crystallization, hydrolysis, washing, calcination and other processes, high-purity white titanium dioxide powder (titanium dioxide) is finally produced.

[0003] The titanium liquid formed after acid dissolution of titanium ore undergoes a series of processes and reaches the hydrolysis process. In the hydrolysis process, precise hydrolysis control is carried out. The titanium oxysulfate in the titanium liquid undergoes a hydrolysis reaction to form solid-phase metatitanic acid, thus completing the key liquid-solid conversion in the production process of titanium dioxide by the sulfuric acid method. This process determines the crystal structure and particle size and other key characteristics of the final product titanium dioxide, and is the most critical process in the production of titanium dioxide by the sulfuric acid method. Before entering the hydrolysis process, the quality of the titanium liquid must be strictly controlled to ensure that the amount of tiny solid impurities that affect the solid conversion result in the titanium liquid is as low as possible. These tiny impurities include impurities brought in from raw materials or the production process, as well as colloidal particles generated by the self-hydrolysis of the titanium liquid. In the existing titanium liquid quality analysis methods, the clarity of the titanium liquid is used to detect the impurities brought in from raw materials or the production process, and the stability of the titanium liquid is used to detect the self-hydrolysis trend of the titanium liquid. However, an analysis method for determining the degree of self-hydrolysis of the titanium liquid itself is rarely applied. The present invention designs an analysis method for the self-hydrolysis degree of titanium liquid to more accurately monitor the quality of titanium liquid. Summary of the Invention

[0004] The purpose of the present invention is to provide an analysis method for the self-hydrolysis degree of titanium liquid, which can simply and quickly determine the self-hydrolysis degree of titanium liquid.

[0005] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0006] An analysis method for the self-hydrolysis degree of titanium liquid includes the following processes:

[0007] S1: Absorb a certain amount of titanium liquid into a beaker, add a certain amount of distilled water under stirring, and record the amount of titanium liquid absorbed as A;

[0008] S2: Keep stirring and record the time B when the solution starts to show white turbidity;

[0009] S3: Let it stand for a certain time, filter the solution by suction filtration, burn the filter paper and the filter residue, weigh it after cooling, and record the weighing value C;

[0010] S4: Using distilled water as the sample, conduct a blank test according to the steps of S1, S2, and S3. It will be subjected to suction filtration, and the filter paper will be burned, cooled, and weighed. Record the weighing value E.

[0011] S5: Calculate the degree of self-hydrolysis D of the titanium solution according to the following formula. The higher the D value, the higher the degree of self-hydrolysis of the titanium solution:

[0012]

[0013] Wherein, the unit of A is milliliters, the unit of B is seconds, and the units of C and E are grams.

[0014] Preferably, in step S1, the amount of titanium solution aspirated is 1 - 10 milliliters.

[0015] When the viscosity of the aspirated titanium solution is relatively high, it is necessary to dilute the titanium solution: Add the aspirated titanium solution to a volumetric flask of a certain volume and dilute it to the mark, and then aspirate a certain amount of the diluted titanium solution for subsequent steps. At this time, the value of A is calculated using the following formula:

[0016]

[0017] Wherein, V1 is the volume of the aspirated titanium solution, with the unit of milliliters; V2 is the volume of the aspirated diluted titanium solution, with the unit of milliliters; V3 is the volume of the volumetric flask, with the unit of milliliters.

[0018] Preferably, in step S1, the amount of distilled water added is 300 - 1000 milliliters.

[0019] Preferably, in step S3, the standing time is 30 - 90 seconds.

[0020] Preferably, in step S3, filtering the solution by suction means transferring the solution into a funnel equipped with 2 layers of precision test paper and conducting suction filtration under a vacuum degree of -0.04 to 0.05 Mpa.

[0021] Preferably, in step S3, burning the filter paper and the filter residue is carried out in an environment of 800 °C.

[0022] Preferably, in step S3, weighing after cooling requires weighing after cooling for at least 30 minutes until constant weight.

[0023] The blank test refers to an operation process in which all the added reagents and operation steps are exactly the same as those for sample determination except that distilled water is used instead of the sample.

[0024] The blank test is carried out simultaneously with the sample test.

[0025] The method provided by the present invention can measure the self-hydrolysis degree of titanium solution, which is simple, rapid and effective, suitable for rapid analysis in the production line, and makes up for the deficiency of the quality analysis of titanium solution. Detailed implementation manners

[0026] In order to make the objectives, technical solutions and advantages of the present invention clearer, the following further describes the present invention in detail with reference to specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, rather than limiting the present invention.

[0027] In order to measure the self-hydrolysis degree of titanium solution, the present invention provides an analysis method for the self-hydrolysis degree of titanium solution, including the following processes:

[0028] S1: Draw 1-10 mL of titanium solution into a 1000 mL beaker, add 300-1000 mL of distilled water under stirring, and record the volume of the drawn titanium solution as A;

[0029] S2: Keep stirring and record the time B when the solution starts to show white turbidity;

[0030] S3: Let it stand for 30-90 seconds, transfer the solution into a funnel with two layers of precision test paper, and perform suction filtration under a vacuum of -0.04 to 0.05 Mpa. Place the filter paper and filter residue in an 800 °C environment for burning, cool for 30 minutes, weigh after constant weight, and record the weighing value;

[0031] S4: Use distilled water as the sample and perform a blank test according to the steps of S1, S2, and S3 (a blank test refers to an operation process in which all the added reagents and operation steps are exactly the same as those in the sample determination except that distilled water is used instead of the sample. The blank test should be carried out simultaneously with the sample determination). It will be subjected to suction filtration, filter paper burning, cooling, and weighing, and record the weighing value E;

[0032] S5: Calculate the self-hydrolysis degree D of the titanium solution at a certain standing time according to the following formula 静置时间 , D 静置时间 The higher the value, the higher the self-hydrolysis degree of the titanium solution:

[0033]

[0034] wherein, A is the volume of the drawn titanium solution, in mL, B is the time when the solution starts to show white turbidity, in s; C is the weight of the filter paper and filter residue after suction filtration and burning, in g; E is the weighing value after burning in the blank test, in g; 1000 is the multiple of converting 1 mL to 1 L; D is the representation of the self-hydrolysis degree of the titanium solution, in g / (L·s), recorded as D 静置时间 , for example, when the standing time is 60 seconds, it is recorded as D 60 .

[0035] Since titanium liquor has a certain viscosity, when the viscosity is too high, directly sucking the titanium liquor for determination will cause a large error. To ensure the accuracy of the analysis, it is necessary to dilute the titanium liquor. For example, when 1 mL of titanium liquor is sampled for determination, due to the high viscosity of this sample, 0.1 mL of the 1 mL of titanium liquor adheres to the sampling instrument and cannot be determined. At this time, the error caused by sampling is -(0.1÷1) = -10%, and this error is unacceptable. To reduce the sampling error, in operation, 10 mL of titanium liquor can be first sucked and diluted to 100 mL, and then 10 mL of the diluted test solution is sucked. At this time, under the same viscosity, even if 0.1 mL of titanium liquor adheres to the sampling instrument, the error caused by sampling is -(0.1÷10) = -1%, and the sampling amount is 10×(10÷100) = 1 mL. After conversion, the sampling amounts are the same, but its accuracy is much higher. Since this is a common operation to reduce sampling error in chemical analysis and is very common, whether to dilute and how much to dilute mainly depends on the requirements of the experiment, and those skilled in the art can determine according to the specific situation of the experiment.

[0036] When the viscosity of the sucked titanium liquor is relatively high, the following method is used to calculate the value of A. Add the sucked titanium liquor into a volumetric flask with a certain volume and dilute it to the scale, and then suck a certain amount of the diluted titanium liquor for subsequent steps. At this time, the value of A is calculated using the following formula:

[0037]

[0038] Among them, V1 is the volume of the sucked titanium liquor, with the unit of mL; V2 is the volume of the sucked diluted titanium liquor, with the unit of mL; V3 is the volume of the volumetric flask, with the unit of mL.

[0039] The following are specific examples.

[0040] Example 1

[0041] S1: Suck 1 mL of titanium liquor into a 1000 mL beaker, and add 500 mL of distilled water while stirring;

[0042] S2: Keep stirring and record the time when the solution starts to show white turbidity;

[0043] S3: Let it stand for 60 seconds, transfer the solution into a funnel with 2 layers of precision test paper, and perform suction filtration under a vacuum degree of -0.04~0.05 Mpa. Place the filter paper and filter residue in an environment of 800 °C for burning, cool for 30 minutes, weigh after constant weight, and record the weighing value;

[0044] S4: Using distilled water as the sample, conduct a blank test according to the steps of S1, S2, and S3 (a blank test refers to an operation process where, except for using distilled water instead of the sample, all other added reagents and operation steps are exactly the same as those for sample determination. The blank test should be carried out simultaneously with the sample determination). It will be subjected to suction filtration, and the filter paper will be burned, cooled, and weighed, and the weighing value E will be recorded;

[0045] S5: Calculate the degree D of the self-hydrolysis of the titanium solution after standing for 60 seconds according to the following formula. The higher the D value, the higher the degree of self-hydrolysis of the titanium solution:

[0046]

[0047] where A is the volume of the titanium solution aspirated, in mL; B is the time when the solution starts to show white turbidity, in seconds; C is the weight of the filter paper and the filter residue after burning after suction filtration, in g; E is the weighing value after burning in the blank test, in g; 1000 is the multiple for converting 1 mL to 1 L; D is the representation of the degree of self-hydrolysis of the titanium solution, in g / (L·s), and is recorded as D 静置时间 , for example, when the standing time is 60 seconds, it is recorded as D 60 .

[0048] Example 2

[0049] S1: Aspirate 10 mL of the titanium solution into a 100 mL volumetric flask, dilute to the mark, and mix well;

[0050] S2: Then aspirate 10 mL of the test solution from the volumetric flask into a 1000 mL beaker, and add 500 mL of distilled water while stirring. Calculate A according to the following formula:

[0051]

[0052] where V1 is the volume of the titanium solution aspirated, in mL; V2 is the volume of the diluted titanium solution taken, in mL; V3 is the volume of the volumetric flask, in mL.

[0053] In this example,

[0054]

[0055] S3: Keep stirring and record the time B when the solution starts to show white turbidity;

[0056] S4: Stand for 60 seconds, transfer the solution into a funnel with 2 layers of precision test paper, conduct suction filtration under a vacuum of -0.04 to -0.05 Mpa, place the filter paper and the filter residue in an 800 °C environment for burning, cool for 30 minutes, and weigh after constant weight, and record the weighing value;

[0057] S5: Use distilled water as the sample and conduct a blank test according to the steps of S1, S2, and S3 (a blank test refers to an operation process in which, except for using distilled water instead of the sample, all other added reagents and operation steps are exactly the same as those for sample determination. The blank test should be carried out simultaneously with the sample determination). It will be subjected to suction filtration, and the filter paper will be burned, cooled, weighed, and the weighing value E will be recorded;

[0058] S6: Calculate the degree of self-hydrolysis of the titanium solution according to the following formula:

[0059]

[0060] where A is the volume of the actual titanium solution after conversion of the diluted test solution, in mL; B is the time when the solution starts to show white turbidity, in seconds; C is the weight of the filter paper and the filter residue after burning after suction filtration, in g; E is the weighing value after burning in the blank test, in g; 1000 is the multiple for converting 1 mL to 1 L; D is the representation of the degree of self-hydrolysis of the titanium solution, in g / (L·s), recorded as D 静置时间 , for example, when the standing time is 60 seconds, it is recorded as D 60 .

[0061] The above specific embodiments describe the basic principles and main features of the present invention. Those skilled in the art of this industry should understand that the protection scope of the present invention is not limited by the above embodiments. Any changes or substitutions that can be thought of without creative labor should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope defined by the claims.

Claims

1. A method for analyzing the self-hydrolysis degree of titanium solution, characterized in that, It includes the following processes: S1: Absorb a certain amount of titanium solution into a beaker, add a certain amount of distilled water while stirring, and record the amount of titanium solution absorbed as A; S2: Keep stirring and record the time B when the solution starts to show white turbidity; S3: Let it stand for a certain time, filter the solution by suction filtration, burn the filter paper and the filter residue, cool it, and then weigh it, and record the weighing value C; S4: Use distilled water as the sample, perform a blank test according to the steps of S1, S2, and S3. It will be filtered by suction filtration, the filter paper will be burned, cooled, and weighed, and record the weighing value E; S5: Calculate the degree of self-hydrolysis D of the titanium solution according to the following formula. The higher the D value, the higher the degree of self-hydrolysis of the titanium solution: Wherein, the unit of A is milliliters, the unit of B is seconds, and the units of C and E are grams.

2. The analysis method for the self-hydrolysis degree of titanium liquid according to claim 1, wherein In step S1, the amount of titanium solution absorbed is 1 - 10 milliliters.

3. The analytical method for the self-hydrolysis degree of titanium solution according to claim 2, characterized in that, When the viscosity of the absorbed titanium solution is relatively high, the titanium solution needs to be diluted: Add the absorbed titanium solution into a volumetric flask with a certain volume and dilute it to the scale, and then absorb a certain amount of the diluted titanium solution for subsequent steps. At this time, the value of A is calculated using the following formula: Wherein, V1 is the volume of the absorbed titanium solution, with the unit of milliliters; V2 is the volume of the absorbed diluted titanium solution, with the unit of milliliters; V3 is the volume of the volumetric flask, with the unit of milliliters.

4. The analytical method for the self-hydrolysis degree of titanium liquid according to claim 1, characterized in that In step S1, the amount of distilled water added is 300 - 1000 milliliters.

5. The analysis method for the self-hydrolysis degree of titanium liquid as described in claim 1, characterized in that, In step S3, the standing time is 30 - 90 seconds.

6. The analysis method of the self-hydrolysis degree of titanium liquid according to claim 1, characterized in that In step S3, filtering the solution by suction filtration means transferring the solution into a funnel with 2 layers of precision test paper and performing suction filtration under a vacuum degree of -0.04 to 0.05 Mpa.

7. The analysis method for the self-hydrolysis degree of titanium liquid as described in claim 1, wherein In step S3, burning the filter paper and the filter residue is carried out in an environment of 800 °C.

8. The analysis method for the self-hydrolysis degree of titanium liquid as described in claim 1, characterized in that, In step S3, weighing after cooling requires weighing after cooling for at least 30 minutes until constant weight.

9. The analysis method for the self-hydrolysis degree of titanium liquid as described in claim 1, characterized in that, The blank test refers to an operation process in which except using distilled water instead of the sample, all other added reagents and operation steps are exactly the same as those for sample determination.

10. The analysis method for the self-hydrolysis degree of titanium solution according to claim 9, characterized in that, The blank test is carried out simultaneously with the sample test.

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