A plasticizing solution for ion liquid regenerated cellulose membrane preparation and a method for detecting silicon content thereof

Abstract

The application discloses a plasticizing liquid for preparing regenerated cellulose membrane from ionic liquid and a detection method for silicon content of the plasticizing liquid, and belongs to the technical field of regenerated cellulose membrane production. The stabilizer is selected from any one of sodium polycarboxylate, sodium polyacrylate or sodium carboxymethyl cellulose. The detection method comprises the following steps: taking the plasticizing liquid into a centrifugal tube, adding a precipitation aid into the plasticizing liquid for reaction, adding a precipitant after the reaction is completed, stirring for a period of time and then standing, then centrifuging, and reserving a silicon-containing solid precipitate; repeatedly washing the silicon-containing solid precipitate with distilled water, drying to obtain a silicon-containing solid, and calculating the content w1 of the silicon-containing solid in the plasticizing liquid according to formula 1. In the application, the stabilizer molecules are adsorbed on the surface of the silica sol particles, the silica sol is prevented from precipitating, the precipitation aid is used to release the silicon dioxide, the silicon dioxide is completely precipitated, and the accuracy of the detection result is remarkably improved.

Description

Technical Field

[0001] This invention relates to the field of regenerated cellulose membrane production technology, specifically to a plasticizing liquid used in the preparation of ionic liquid regenerated cellulose membranes and a method for detecting its silicon content. Background Technology

[0002] Ionic liquid regenerated cellulose membrane is a fully biodegradable green film material made from natural cellulose through solvent-based gelation, followed by multiple processes including film spraying, washing, plasticizing, and drying. It is widely used in food packaging, tobacco packaging, gift packaging, labeling, and specialty packaging. The silica sol in the plasticizing solution is an anionic colloid, mainly composed of silica particles with a negatively charged surface. It forms an electric double layer by adsorbing counterions, and the particles remain stable due to electrostatic repulsion. When solvent-produced cellulose membranes pass through the plasticizing solution, ionic liquid may enter the solution. This entry of ionic liquid can easily cause silica sol precipitation, adversely affecting the silica sol coating effect and impacting the anti-sticking properties of the ionic liquid regenerated cellulose membrane.

[0003] Furthermore, in the production line of ionic liquid regenerated cellulose membranes, the cellulose membrane continuously passes through a plasticizing liquid, carrying away the silica sol in the plasticizing liquid. This reduces the concentration of silica in the silica sol, and the change in concentration directly affects the amount of silica sol applied, thus affecting the storage time and quality of the finished regenerated cellulose membrane. Therefore, it is necessary to periodically monitor and control the concentration of silica sol in the plasticizing liquid. Currently, methods for detecting silica sol concentration generally employ the density conversion method (GB / T4472-2011) or the method using methyl red-bromocresol green as a colorimetric reagent, treated with concentrated sulfuric acid, and then titrated with sodium hydroxide. However, these methods cannot accurately detect silica sol concentration in mixtures containing other impurities or in solutions that easily turn red, such as red cellulose membranes. While the ignition constant-weight method (GB / T 18174, GB / T 4209) and the drying and weighing method can accurately detect silica sol concentration, they are time-consuming and unsuitable for continuous cellulose membrane production systems.

[0004] In view of the problems existing in the prior art, the present invention combines the relevant characteristics of ionic liquids and silica sols to design a plasticizing liquid for the preparation of ionic liquid regenerated cellulose membranes and a method for detecting its silicon content, so as to overcome the above defects. Summary of the Invention

[0005] To address the problems existing in the prior art, this invention provides a method for detecting the silicon content of a plasticizing solution used in the preparation of ionic liquid regenerated cellulose membranes. This method avoids the influence of ionic liquids on silica sol, improves the stability of the plasticizing solution, and benefits the plasticizing effect of the regenerated cellulose membrane. By using a settling agent to release silica particles stabilized by a stabilizer, and then using a precipitant to settle the silica, the amount of silica can be calculated, thereby improving the accuracy of silica content detection.

[0006] To achieve the above objectives, on the one hand, the present invention provides a plasticizing solution for the preparation of ionic liquid regenerated cellulose membranes, the plasticizing solution comprising an aqueous glycerol solution, an aqueous silica sol solution, and a stabilizer; The stabilizer is selected from any one of sodium polycarboxylate aqueous solution, sodium polyacrylate aqueous solution, or sodium carboxymethyl cellulose aqueous solution; The concentration of the glycerol aqueous solution is 50-80 g / L, and the dosage is 130-160 kg / ton of membrane. The silica sol aqueous solution contains 1.5-2.5 g / L of silica, and the dosage is 0.3-0.4 kg / ton of membrane. The stabilizer concentration is 1-3 g / L, and the dosage is 0.05-0.1 kg / ton of membrane.

[0007] This invention also provides a method for detecting the silicon content in plasticizing liquids, comprising the following steps: S1, take the plasticized liquid into a centrifuge tube, and add a settling agent to the plasticized liquid to react; S2, after the reaction is complete, add the precipitant, stir for a period of time and let stand, then centrifuge and retain the silicon-containing solid precipitate; S3, repeatedly wash the silicon-containing solid precipitate with distilled water, dry it to obtain silicon-containing solid, and calculate the content w1 of silicon-containing solid in plasticized liquid according to formula 1; Formula 1; in, To determine the mass of the plasticizing liquid, For the mass of empty centrifuge tubes, The total mass of the silicon-containing solids and centrifuge tubes is given by A, which is the blank coefficient of the plasticized liquid. The settling agent is selected from any one of polyacrylamide solution, polyethyleneimine solution, and dodecyltrimethylammonium hydroxide solution.

[0008] Preferably, the reaction temperature in step S1 is 50-60℃ and the reaction time is 5-10 min.

[0009] Preferably, the precipitant is selected from any one of polyaluminum chloride solution, polyaluminum sulfate solution, polyferric chloride solution, and polyferric sulfate solution.

[0010] Preferably, the ratio of the mass (g) of the plasticizing liquid to the volume (mL) of the precipitant is (4-5):(1-2). The ratio of the mass g of the plasticized liquid to the volume mL of the settling agent is (8-10):(1-2).

[0011] Preferably, the stirring time in step S2 is 10-20 min and the centrifugation speed is 4000 r / min.

[0012] Preferably, the mass concentration of the precipitant is 1-5%; The mass concentration of the settling agent is 1-5%.

[0013] Preferably, the drying temperature in step S3 is 105-115℃ and the drying time is 2-3 hours.

[0014] Preferably, the plasticizer blank coefficient A is obtained according to the following steps: T1. Prepare a blank glycerol solution in a centrifuge tube according to the concentration of glycerol in the plasticized liquid, and add a flocculant to the blank glycerol solution to react. T2, after the reaction is complete, add the precipitant, stir for a period of time and then centrifuge to retain the solid precipitate; T3, wash the solid precipitate repeatedly with distilled water, dry it to obtain the insoluble substance, and calculate the blank coefficient A of the plasticized liquid according to formula 2; Formula 2; in, To determine the mass of the plasticizing liquid, For the mass of empty centrifuge tubes, The total mass of the insoluble substances and the centrifuge tube; The mass of the glycerol blank solution is equal to the mass of the plasticized liquid weighed.

[0015] The advantages of this invention are: 1. This invention uses an anionic polymeric dispersant as a stabilizer in the plasticizing solution. By utilizing the electrostatic stabilization mechanism, the stabilizer molecules carry a negative charge and adsorb onto the surface of silica sol particles, thereby increasing the absolute value of the Zeta potential, enhancing the electrostatic repulsion force, and preventing silica sol from precipitating and affecting the plasticizing effect of the cellulose membrane.

[0016] 2. This invention breaks the balance between the stabilizer and the silica sol by adding a flocculant. The positive charge of the flocculant strongly neutralizes the negative charge on the surface of the silica sol particles and the residual negative charge in the stabilizer molecules (in the system), quickly eliminating electrostatic repulsion and causing the colloidal system to lose stability. Subsequently, the silica sol is completely precipitated under the action of the precipitant, improving the accuracy of silica content detection. Attached Figure Description

[0017] Figure 1A comparison of the state of the plasticized liquid after adding a stabilizer and then adding an ionic liquid (left side) and the state after not adding a stabilizer and then adding an ionic liquid (right side). Detailed Implementation

[0018] To facilitate understanding by those skilled in the art, the present invention will be further described below with reference to specific embodiments.

[0019] This invention provides a plasticizing solution for preparing ionic liquid regenerated cellulose membranes. The plasticizing solution comprises an aqueous glycerol solution, an aqueous silica sol solution, and a stabilizer. The aqueous glycerol solution has a concentration of 50-80 g / L and is used at a dosage of 130-160 kg / ton of membrane. The silica sol solution has a silica content of 1.5-2.5 g / L and is used at a dosage of 0.3-0.4 kg / ton. The stabilizer has a concentration of 1-3 g / L and is used at a dosage of 0.05-0.1 kg / ton of membrane. The stabilizer is selected from any one of an aqueous solution of sodium polycarboxylate, an aqueous solution of sodium polyacrylate, or an aqueous solution of sodium carboxymethyl cellulose.

[0020] In the ionic liquid cellulose membrane production line, to prevent the ionic liquid from entering the plasticizing liquid and causing silica sol precipitation, this invention adds a stabilizer to the plasticizing liquid. The stabilizer is adsorbed on the surface of the silica sol particles, increasing the absolute value of the zeta potential and enhancing the electrostatic repulsion force to keep the silica sol stable, ensuring the normal progress of the film plasticizing process and ensuring the quality of the cellulose membrane.

[0021] The present invention also provides a method for detecting the silicon content in the above-mentioned plasticizing liquid, comprising the following steps: S1, take the plasticized liquid into a centrifuge tube, add a settling agent to the plasticized liquid and react. The reaction temperature is 50-60℃ and the reaction time is 5-10min. S2, after the reaction is complete, add the precipitant, stir for 10-20 minutes and let stand, then centrifuge at 4000 r / min to retain the silicon-containing solid precipitate; S3, repeatedly wash the silicon-containing solid precipitate with distilled water, dry it at 105-115℃ for 2-3 hours to obtain silicon-containing solid, and calculate the content w1 of silicon-containing solid in plasticized liquid according to formula 1; Formula 1; in, To determine the mass of the plasticizing liquid, For the mass of empty centrifuge tubes, A represents the total mass of the silicon-containing solids and centrifuge tubes, and A is the blank coefficient of the plasticized liquid.

[0022] The settling aid is selected from any one of polyacrylamide solution, polyethyleneimine solution, and dodecyltrimethylammonium hydroxide solution. The precipitant is selected from any one of polyaluminum chloride solution, polyaluminum sulfate solution, polyferric chloride solution, and polyferric sulfate solution. The mass ratio (g) of the plasticized liquid to the volume (mL) of the precipitant is (4-5):(1-2), the mass ratio (g) of the plasticized liquid to the volume (mL) of the settling aid is (8-10):(1-2), the mass concentration of the precipitant is 1-5%, and the mass concentration of the settling aid is 1-5%.

[0023] In the plasticized liquid system of this invention, when determining the silica content using the precipitation method, the presence of stabilizers in the plasticized liquid prevents all silica from precipitating out, thus affecting the accuracy of the test results. This invention utilizes the characteristics of silica sol as anionic colloids and stabilizers as mostly anionic polymeric dispersants. By adding a cationic aqueous polymer as a flocculant to the plasticized liquid, the positive charge of the flocculant strongly neutralizes the negative charge on the surface of the silica sol particles and the residual negative charge of the stabilizer molecules, rapidly eliminating electrostatic repulsion and causing the colloidal system to lose stability. Finally, under the action of the precipitant, the silica is completely precipitated. In this invention, the precipitant hydrolyzes in water to generate polynuclear hydroxyl complex ions, which mainly precipitate silica through charge neutralization, completely destroying the colloidal stability.

[0024] Because some glycerol in the plasticizing liquid will also precipitate under the action of the precipitant, causing the test results to deviate from the correct value, the present invention prepares an aqueous solution of glycerol with the same concentration as that in the plasticizing liquid, i.e., a glycerol blank solution, and determines the mass content of the solid precipitate finally obtained in the glycerol blank solution according to the above-mentioned detection method of silica content, which is used as the plasticizing liquid blank coefficient A, to eliminate the influence of glycerol and other solid impurities and improve the accuracy of the test results.

[0025] The blank coefficient A of the plasticized liquid is obtained by the following steps: T1. Prepare a blank glycerol solution in a centrifuge tube according to the concentration of glycerol in the plasticized solution. Add a flocculant to the blank glycerol solution and react at 50-60℃ for 5-10 minutes. T2, after the reaction is complete, add the precipitant, stir for 10-20 minutes and then centrifuge at 4000 r / min, retaining the solid precipitate; T3, wash the solid precipitate repeatedly with distilled water, dry it to obtain the insoluble substance, and calculate the blank coefficient A of the plasticized liquid according to formula 2; Formula 2; in, To determine the mass of the plasticizing liquid, For the mass of empty centrifuge tubes, This is the total mass of the insoluble substances and the centrifuge tubes.

[0026] The mass ratio of the blank glycerol solution (g) to the volume ratio of the precipitant (mL) is (4-5):(1-2), and the mass ratio of the blank glycerol solution (g) to the volume ratio of the precipitant (mL) is (8-10):(1-2).

[0027] The specific implementation method is as follows:

[0028] Unless otherwise specified, the experimental methods used in this invention are all conventional methods, and the materials and reagents used are all commercially available unless otherwise specified.

[0029] Example 1 A plasticizing solution for preparing ionic liquid regenerated cellulose membranes comprises an aqueous glycerol solution with a concentration of 68 g / L and a dosage of 149.2 kg / ton of membrane, an aqueous silica sol solution with a silica content of 1.8 g / L and a dosage of 0.32 kg / ton of membrane, and a sodium polycarboxylate stabilizer with a concentration of 2.5 g / L and a dosage of 0.09 kg / ton of membrane.

[0030] Example 2 A plasticizing solution for preparing ionic liquid regenerated cellulose membranes comprises an aqueous glycerol solution with a concentration of 54 g / L and a dosage of 130 kg / ton of membrane, an aqueous silica sol solution with a silica content of 2.0 g / L and a dosage of 0.35 kg / ton of membrane, and a sodium polyacrylate stabilizer with a concentration of 1.5 g / L and a dosage of 0.06 kg / ton of membrane.

[0031] Example 3

[0032] A plasticizing solution for preparing ionic liquid regenerated cellulose membranes comprises an aqueous glycerol solution with a concentration of 72 g / L and a dosage of 158 kg / ton of membrane, an aqueous silica sol solution with a silica content of 2.3 g / L and a dosage of 0.38 kg / ton of membrane, and a sodium carboxymethyl cellulose stabilizer with a concentration of 2.0 g / L and a dosage of 0.08 kg / ton of membrane.

[0033] Experimental Example 1 This test example detects the silica content in the plasticized liquid of Example 1; The blank coefficient A of the plasticized liquid is obtained by the following steps: T1. Prepare a glycerol blank solution in a centrifuge tube according to the concentration of glycerol in the plasticized liquid, and weigh 49.9952g. Add 5 mL of 3% polyacrylamide solution as a flocculant to the glycerol blank solution and react at 50℃ for 10 min. T2, after the reaction is complete, add 20 mL of polyaluminum chloride solution as a precipitant and stir for 15 min. Then centrifuge at 4000 r / min for 5 min, remove the supernatant and retain the solid precipitate. T3. Add 45 mL of distilled water to the centrifuge tube and wash the solid precipitate repeatedly. Place the centrifuge tube with the precipitate in an oven at 110°C and dry it for 3 hours to obtain the insoluble substance. Calculate the blank coefficient A of the plasticized liquid according to Formula 2. Formula 2; Determination of silica content: S1, take 50g of plasticized liquid into a centrifuge tube, add 5 mL of 3% polyacrylamide solution as a flocculant to the plasticized liquid, and react at 50℃ for 10 min; S2, after the reaction is complete, add 20 mL of polyaluminum chloride solution as a precipitant and stir for 15 min. Then centrifuge at 4000 r / min for 5 min, remove the supernatant and retain the silicon-containing solid precipitate. S3. Add 45 mL of distilled water to the centrifuge tube and wash the silicon-containing solid precipitate repeatedly. Place the centrifuge tube with the precipitate in an oven at 110°C and dry it for 3 hours to obtain silicon-containing solid. Calculate the content w1 of silicon-containing solid in the plasticized liquid according to Formula 1. Formula 1; Three experiments were conducted following the steps described above, and the average value of the test results was taken, as shown in Table 1.

[0034] Experimental Example 2 This test example detects the silica content in the plasticized liquid of Example 2; The blank coefficient A of the plasticized liquid is obtained by the following steps: T1. Prepare a glycerol blank solution in a centrifuge tube according to the concentration of glycerol in the plasticized liquid, and weigh 49.9964g. Add 5 mL of 3% polyethyleneimine solution as a flocculant to the glycerol blank solution and react at 50℃ for 10 min. T2, after the reaction is complete, add 20 mL of polyaluminum sulfate solution as a precipitant and stir for 10 min. Then centrifuge at 4000 r / min for 5 min, remove the supernatant and retain the solid precipitate. T3. Add 45 mL of distilled water to the centrifuge tube and wash the solid precipitate repeatedly. Place the centrifuge tube with the precipitate in an oven at 110°C and dry it for 3 hours to obtain the insoluble substance. Calculate the blank coefficient A of the plasticized liquid according to Formula 2. Formula 2; Determination of silica content: S1, take 50g of plasticized liquid into a centrifuge tube, add 5 mL of 3% polyethyleneimine solution as a flocculant to the plasticized liquid, and react at 50℃ for 10 min; S2, after the reaction is complete, add 20 mL of polyaluminum sulfate solution as a precipitant and stir for 10 min. Then centrifuge at 4000 r / min for 5 min, remove the supernatant and retain the silicon-containing solid precipitate. S3. Add 45 mL of distilled water to the centrifuge tube and wash the silicon-containing solid precipitate repeatedly. Place the centrifuge tube with the precipitate in an oven at 110°C and dry it for 3 hours to obtain silicon-containing solid. Calculate the content w1 of silicon-containing solid in the plasticized liquid according to Formula 1. Formula 1; Three experiments were conducted following the steps described above, and the average value of the test results was taken, as shown in Table 1.

[0035] Experimental Example 3 This test example detects the silica content in the plasticized liquid of Example 3; The blank coefficient A of the plasticized liquid is obtained by the following steps: T1. Prepare a blank glycerol solution in a centrifuge tube according to the concentration of glycerol in the plasticized liquid, and weigh 49.9984 g. Add 5 mL of 3% dodecyltrimethylammonium hydroxide solution as a flocculant to the blank glycerol solution and react at 50℃ for 10 min. T2, after the reaction is complete, add 20 mL of polyferric chloride solution as a precipitant and stir for 20 min. Then centrifuge at 4000 r / min for 5 min, remove the supernatant and retain the solid precipitate. T3. Add 45 mL of distilled water to the centrifuge tube and wash the solid precipitate repeatedly. Place the centrifuge tube with the precipitate in an oven at 110°C and dry it for 3 hours to obtain the insoluble substance. Calculate the blank coefficient A of the plasticized liquid according to Formula 2. Formula 2; Determination of silica content: S1, take 50g of plasticized liquid into a centrifuge tube, add 5 mL of 3% dodecyltrimethylammonium hydroxide solution as a flocculant to the plasticized liquid, and react at 50℃ for 10 min; S2, after the reaction is complete, add 20 mL of polyferric chloride solution as a precipitant and stir for 20 min. Then centrifuge at 4000 r / min for 5 min, remove the supernatant and retain the silicon-containing solid precipitate. S3. Add 45 mL of distilled water to the centrifuge tube and wash the silicon-containing solid precipitate repeatedly. Place the centrifuge tube with the precipitate in an oven at 110°C and dry it for 3 hours to obtain silicon-containing solid. Calculate the content w1 of silicon-containing solid in the plasticized liquid according to Formula 1. Formula 1; Three experiments were conducted following the steps described above, and the average value of the test results was taken, as shown in Table 1.

[0036] Comparative Example 1 The comparative example measures the silica content in the plasticized liquid of Example 1 according to the steps of Experimental Example 1. The difference is that in this comparative example, after weighing the glycerol blank solution in step T1, the precipitant is added directly, omitting the flocculant; after weighing the plasticized liquid in step S1, the precipitant is added directly, omitting the flocculant.

[0037] Comparative Example 2 The comparative example prepared the plasticizing liquid according to the steps of Example 1, except that the plasticizing liquid did not include a 2.5 g / L concentration of sodium polycarboxylate stabilizer solution.

[0038] Plasticized liquid stability test: Ionic liquids (ILs) were added dropwise to the plasticizing solutions of Example 1 and Comparative Example 2 to simulate the effect of ILs on plasticizing solutions in actual production, and the states of the two solutions were observed. Figure 1 The left side shows the state diagram of the plasticizing liquid after adding IL in Example 1. Figure 1 The right side shows the state diagram of the plasticized liquid in Comparative Example 2 after adding IL. It can be clearly seen from the figure that the plasticized liquid in Comparative Example 2 without the addition of stabilizer is layered, with the upper layer being a transparent clear liquid and the lower layer being a white precipitate of silica. In this invention, the stabilizer can effectively improve the stability of the plasticized liquid.

[0039] Table 1 shows the silicon content test results for Test Examples 1-3 and Comparative Example 1. The average silicon content in Table 1 is the average of the results obtained from three tests for one test example. The standard value is the actual silicon dioxide content in the plasticizing liquid used in that test example.

[0040] Table 1. Detection results of silica content in different samples

[0041] As shown in Table 1, the silica content measured in Examples 1-3 is comparable to the actual silica content in the plasticizing liquid, indicating that the detection method of the present invention can accurately measure the silica content in the plasticizing liquid. This allows for real-time measurement of silica concentration during production, ensuring the anti-adhesion effect of the cellulose membrane. Comparing the results of Comparative Example 1 with those of Example 1 shows that the flocculant in the present invention successfully disrupts the stability of silica sol in the plasticizing liquid system, thereby allowing silica and glycerol to precipitate completely in subsequent processes, ensuring the accuracy of the detection results.

[0042] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of protection of the invention. Furthermore, it should be understood that after reading the technical description of this invention, those skilled in the art can make various alterations, modifications, and / or variations to the invention, and all such equivalent forms also fall within the scope of protection defined by the appended claims.

Claims

1. A plasticizing solution for preparing ionic liquid regenerated cellulose membranes, characterized in that, The plasticizing solution comprises an aqueous glycerol solution, an aqueous silica sol solution, and a stabilizer; The stabilizer is selected from any one of sodium polycarboxylate aqueous solution, sodium polyacrylate aqueous solution, or sodium carboxymethyl cellulose aqueous solution; The concentration of the glycerol aqueous solution is 50-80 g / L, and the dosage is 130-160 kg / ton of membrane. The silica sol aqueous solution contains 1.5-2.5 g / L of silica, and the dosage is 0.3-0.4 kg / ton of membrane. The stabilizer concentration is 1-3 g / L, and the dosage is 0.05-0.1 kg / ton of membrane.

2. A method for detecting the silicon content in the plasticizing liquid as described in claim 1, characterized in that, Includes the following steps: S1, take the plasticized liquid into a centrifuge tube, and add a settling agent to the plasticized liquid to react; S2, after the reaction is complete, add the precipitant, stir for a period of time and let stand, then centrifuge and retain the silicon-containing solid precipitate; S3, repeatedly wash the silicon-containing solid precipitate with distilled water, dry it to obtain silicon-containing solid, and calculate the content w1 of silicon-containing solid in plasticized liquid according to formula 1; Formula 1; in, To determine the mass of the plasticizing liquid, For the mass of empty centrifuge tubes, The total mass of the silicon-containing solids and centrifuge tubes is given by A, which is the blank coefficient of the plasticized liquid. The settling aid is selected from any one of polyacrylamide solution, polyethyleneimine solution, and dodecyltrimethylammonium hydroxide solution; The blank coefficient A of the plasticized liquid is obtained by the following steps: T1. Prepare a blank glycerol solution in a centrifuge tube according to the concentration of glycerol in the plasticized liquid, and add a flocculant to the blank glycerol solution to react. T2, after the reaction is complete, add the precipitant, stir for a period of time and let stand, then centrifuge and retain the solid precipitate; T3, wash the solid precipitate repeatedly with distilled water, dry it to obtain the insoluble substance, and calculate the blank coefficient A of the plasticized liquid according to formula 2; Formula 2; in, To determine the mass of the plasticizing liquid, For the mass of empty centrifuge tubes, The total mass of the insoluble substances and the centrifuge tube; The mass of the glycerol blank solution is equal to the mass of the plasticized liquid weighed.

3. The method for detecting silicon content in plasticizing liquid according to claim 2, characterized in that, In step S1, the reaction temperature is 50-60℃ and the reaction time is 5-10 min.

4. The method for detecting silicon content in plasticizing liquid according to claim 2, characterized in that, The precipitant is selected from any one of polyaluminum chloride solution, polyaluminum sulfate solution, polyferric chloride solution, and polyferric sulfate solution.

5. The method for detecting silicon content in plasticizing liquid according to claim 2, characterized in that, The ratio of the mass (g) of the plasticized liquid to the volume (mL) of the precipitant is (4-5):(1-2). The ratio of the mass g of the plasticized liquid to the volume mL of the settling agent is (8-10):(1-2).

6. The method for detecting silicon content in plasticizing liquid according to claim 2, characterized in that, In step S2, the stirring time is 10-20 min and the centrifugation speed is 4000 r / min.

7. The method for detecting silicon content in plasticizing liquid according to claim 2, characterized in that, The mass concentration of the precipitant is 1-5%; The mass concentration of the settling agent is 1-5%.

8. The method for detecting silicon content in plasticized liquid according to claim 2, characterized in that, In step S3, the drying temperature is 105-115℃ and the drying time is 2-3 hours.

Images