CN112326383B - Modified nano SiO2 water quality processor turbidity labeling substance and preparation method thereof - Google Patents
Modified nano SiO2 water quality processor turbidity labeling substance and preparation method thereof Download PDFInfo
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- CN112326383B CN112326383B CN202011190006.1A CN202011190006A CN112326383B CN 112326383 B CN112326383 B CN 112326383B CN 202011190006 A CN202011190006 A CN 202011190006A CN 112326383 B CN112326383 B CN 112326383B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N2001/2893—Preparing calibration standards
Abstract
The invention belongs to the technical field of standard substance preparation, and relates to modified nano SiO 2 Water quality processorTurbidity adding material and its preparation process. The added standard substance is modified nano SiO subjected to modification treatment 2 Said SiO 2 Is spherical particle with average particle diameter of 100-500nm. The invention reduces the nanometer SiO by modifying the 3-chloropropyltrimethoxysilane and the hydrochloric acid under the synergistic action 2 The acting force between the surface hydroxyl groups forms a clear particle surface to prevent the nano SiO 2 The agglomeration and the standing stability are good. The modified nano SiO prepared by the invention 2 The concentration of the solution has a better linear relation with the turbidity, and the solution has the characteristic of being used as a turbidity adding standard substance of the water quality processor. And can prepare modified nano SiO with different particle diameters according to the requirements of filter elements with different precisions 2 The aqueous solution has good particle size controllability. The modified nano SiO prepared by the invention 2 The solution has no influence on oxygen consumption and pH value of water.
Description
Technical Field
The invention belongs to the technical field of standard substance preparation, and particularly relates to modified nano SiO 2 A turbidity labeling substance of a water quality processor and a preparation method thereof.
Background
Turbidity is an important physical index for representing the turbidity degree of water quality. The turbidity of source water is due to scattering or absorption behavior in optical terms caused by suspended or colloidal matter, or both. The household and similar water purifier can eliminate the surface water pollution, the by-product of tap water disinfection and the secondary pollution of water pipeline to the drinking water of residents. In order to standardize the inspection work of the sanitary and safe products of the drinking water and strengthen the supervision and management on the quality of the water quality processor, the Ministry of health establishes the inspection regulation of the sanitary department on the sanitary and safe products of the drinking water in 2001. The turbidity is required to be detected in the sanitary safety and sanitary functional tests of water delivery and distribution equipment (pipes, pipe fittings, water storage containers and water stop materials), protective materials (coatings, linings and the like), water treatment materials and general water quality processors which are required to be in contact with the drinking water. The turbidity standard adding experiment is required for the common water quality processor of the activated carbon filter element and the membrane filtration component, but the turbidity standard adding substance and the configuration method thereof are not indicated in the specification. Different labeling objects are selected by each detection mechanism when a general water quality processor is used for turbidity detection according to the inspection regulations of sanitary products related to drinking water sanitation safety of Ministry of health, so that the detection results have larger difference and objective judgment on the performance of the water quality processor cannot be made. The national standard QB/T4143-2019 published by the Ministry of industry and belief in China, "general water quality processor for household and similar applications" and QB/T4144-2019, "pure water processor for household and similar applications" stipulate that a formalin solution of 25 NTU is used as a water quality processor and a standard substance for turbidity test of the pure water processor. Since the formalin suspension is an unstable suspension system as an inhomogeneous suspension system, there are obvious disadvantages in the use process.
Formalin turbidity standard is the standard of turbidity commonly used. The difference of environmental temperature in the preparation process can cause the difference of particle size, and the difference of the temperature of the placing time and the placing environment can cause the particle size to be changed continuously, thus causing the particle size of the formalin in the suspension to be uncontrollable. Because the particle diameter of the formalin solution is larger and the sedimentation speed is high, after the formalin solution is placed for a period of time, the particles in the formalin solution can be sedimentated to form larger concentration difference, and the defect of poor standing stability exists. The ideal standard substance required in the standard addition experiment of the water quality processor can not change other physicochemical indexes of water quality except that the concentration of the standard substance reaches the standard requirement, and simultaneously has certain stability and reasonable turbidity removal rate. In the prior art, no relevant record exists for modifying silicon dioxide to be used as a turbidity adding substance of a water quality processor.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a modified nano SiO 2 The turbidity of the water quality processor is added with a standard substance.
The invention also provides a modified nano SiO 2 A preparation method of a turbidity adding standard substance of a water quality processor.
The technical scheme adopted by the invention for realizing the purpose is as follows:
the invention provides a modified nano SiO 2 A turbidity labeling substance of the water quality processor, the SiO 2 Is spherical particle with average particle diameter of 100-500nm.
The invention also provides a modified nano SiO 2 The preparation method of the turbidity standard substance of the water quality processor is characterized by comprising the following steps:
(1) Weighing nano SiO 2 Dissolving in absolute ethyl alcohol, performing ultrasonic oscillation, and performing magnetic stirring to obtain silicon dioxide ethanol solution for later use;
(2) Adding 3-chloropropyltrimethoxysilane into the dispersed nano SiO 2 Performing constant-temperature water bath reaction in an ethanol solution, adding a proper amount of hydrochloric acid with the volume concentration of 3%, continuously reacting, continuously stirring in the reaction process, after the reaction is finished, performing centrifugal separation, washing for 3 times by using absolute ethyl alcohol, performing vacuum drying, and weighing a proper amount of modified nano SiO 2 Adding tertiary water into the powder, and ultrasonically dispersing the powder by 1h to prepare a standard solution.
Further, in the step (1), the nano SiO 2 The ratio of the ethanol to the absolute ethyl alcohol is 1g:30mL.
Further, in the step (1), the time for ultrasonic oscillation and magnetic stirring is 60min.
Further, in the step (2), the 3-chloropropyltrimethoxysilane and the nano SiO 2 The mass ratio of (A) is 2-3:1.
In the preparation method provided by the invention, the constant-temperature water bath reaction is carried out for 0.5h at 85 ℃.
Further, the addition amount of the hydrochloric acid is 1g of nano SiO 2 1mL of the solution was added.
In the reaction process, after a proper amount of 3% hydrochloric acid is added, the reaction is continued for 3.5h.
Further, the vacuum drying is drying at 55 ℃ for 8h.
The invention also provides the nano SiO prepared by the preparation method 2 As a water processor for turbidity plusThe application of the target substance.
The invention selects the nano silicon dioxide powder with controllable grain diameter as a matrix, improves the dispersibility and stability of the nano silicon dioxide powder in aqueous solution by modifying the nano silicon dioxide powder by organosilane, and simultaneously discusses SiO by comparing a formalin added standard substance and modified nano 2 The influence of the aqueous solution on the oxygen consumption and the pH value of water quality has more excellent performance as a turbidity adding substance of a water quality processor.
The invention has the beneficial effects that:
(1) The invention successfully and covalently combines the modifier to the nano SiO under the synergistic action of 3-chloropropyltrimethoxysilane and hydrochloric acid 2 Surface, reduced nano SiO 2 The acting force between the surface hydroxyl groups forms a clear particle surface to prevent the nano SiO 2 The agglomeration and the standing stability are good.
(2) The modified nano SiO prepared by the invention 2 The concentration of the solution has a better linear relation with the turbidity degree, and the correlation coefficient R 2 0.9995; modified nano SiO 2 The solution has better dilution characteristic and linear relation to the correlation coefficient R 2 Is 0.9979. Modified nano SiO 2 The aqueous solution has better stability and dilution characteristics, has higher linear relation between the concentration and the turbidity, and has the characteristic of serving as a turbidity adding standard substance of the water quality processor. And modified nano SiO with different grain diameters can be prepared according to the requirements of different filtering membranes 2 The aqueous solution has good particle size controllability.
(3) The modified nano SiO prepared by the invention 2 The solution does not affect the oxygen consumption and the pH value of the water quality.
Drawings
FIG. 1 shows the nano SiO before and after modification of 3-chloropropyltrimethoxysilane prepared in example 1 2 SEM picture of (1);
wherein, (a) unmodified nano SiO 2 (b) modified nano SiO 2 。
FIG. 2 shows a view of nano SiO 2 Infrared spectra before and after modification with 3-chloropropyltrimethoxysilane;
wherein 1: is not modified; 2: only 3-chloropropyltrimethoxysilane is used for modification; 3:3-chloropropyltrimethoxysilane was synergistically modified with HCL.
FIG. 3 preparation of nano SiO in example 1 2 Particle size distribution diagram of (c).
FIG. 4 is a particle size distribution diagram of a Formazin solution.
FIG. 5 is a graph of the trend of Formazin solution Dav over time.
FIG. 6 shows modified nano SiO 2 Trend plot of solution Xav over time.
FIG. 7 shows modified nano SiO 2 Turbidity value of aqueous solution.
FIG. 8 shows modified nano SiO 2 Dilution profile of aqueous solution.
FIG. 9 shows modified nano SiO 2 Standing the solution (412 NTU) and the Formazin solution (400 NTU).
FIG. 10 shows modified nano SiO 2 The turbidity of the solution and the Formazin solution changes.
Detailed Description
The technical solution of the present invention is further explained and illustrated by the following specific examples.
Reagents and instruments used in the invention:
reagent: nano SiO 2 (Shanghai Changbai nanometer materials science and technology Co., ltd., average particle diameter of 100-500 nm), 3-chloropropyltrimethoxysilane (Aladdin reagent Co., ltd.), absolute ethyl alcohol (analytical pure AR of national drug group chemical reagent Co., ltd.), hydrochloric acid (premium grade pure GR of national drug group chemical reagent Co., ltd.)
The instrument comprises: magnetic control stirring heater (Sijin Seidelis test analyzer manufacturing factory), analytical balance (Sidolis Scientific instruments (Beijing) Co., ltd.), fourier transform micro infrared spectrometer (Thermo Scientific), scatterometer (Shanghai Xinrui instruments and meters Co., ltd.), centrifuge (Hunan instruments and meters Co., ltd. In the development area of Changsha high tech industry), vacuum drying oven (Shanghai Bingshi industries Co., ltd.), digital display constant temperature water bath (Changzhou Nuoji instruments Co., ltd.), and standard light source box (tin source box)Ley-altalas limited), a nanoparticle size analyzer Winner802 (denna micro-nano particle technology limited), a laser particle size analyzer Winner2000ZD (denna micro-nano particle technology limited), a thermal field emission scanning electron microscope SUPPA TM 55 (Zeiss, germany).
Example 1
Weighing 2g of nano SiO 2 Dissolving in 60mL of absolute ethyl alcohol, ultrasonically shaking for 60min, and magnetically stirring for 1h. Adding 4.324g 3-chloropropyltrimethoxysilane into the dispersed nano SiO 2 In the ethanol solution, after 0.5h reacts in a thermostatic waterbath at 85 ℃, 2mL of 3% hydrochloric acid is added, the reaction is continued for 3.5h, the stirring is continuously carried out in the reaction process, after the reaction is finished, the centrifugal separation is carried out for 15min, and the absolute ethyl alcohol is used for washing for 3 times. Drying 8h in 55 deg.C vacuum drying oven, grinding into powder, and weighing appropriate amount of modified nanometer SiO 2 Adding three-stage water into the powder, ultrasonically dispersing the powder for 1h, and preparing a standard stock solution with a certain turbidity of about 400 NTU.
Comparative example 1
Weighing 2g of nano SiO 2 Dissolving in 60mL of absolute ethyl alcohol, ultrasonically shaking for 60min, and magnetically stirring for 1h. Adding 4 mL of 3-chloropropyltrimethoxysilane into the dispersed nano SiO 2 Reacting in ethanol solution in a constant temperature water bath at 85 ℃ for 4h, continuously stirring in the reaction process, centrifugally separating for 15min after the reaction is finished, and washing with absolute ethyl alcohol for 3 times. Drying in a vacuum drying oven at 55 deg.C for 8 hr, grinding into powder, and weighing appropriate amount of modified nanometer SiO 2 Adding three-stage water into the powder, ultrasonically dispersing the powder by 1h, and preparing a standard solution with certain turbidity.
Results and discussion
(one) the 3-chloropropyltrimethoxysilane prepared in example 1 is modified to prepare nano SiO 2 Is shown in fig. 1. As can be seen from FIG. 1, the unmodified nano SiO 2 The particles exist in an agglomerated form due to stronger acting force of hydroxyl groups among the particles, so that the surfaces of the particles are not obvious, and 3-chloropropyltrimethoxysilane is cooperated with hydrochloric acid to modify SiO 2 The introduction of the middle hydrophobic group reduces the nano SiO 2 The force between the surface hydroxyl groups forms a clear particle surface.
(II) modifying SiO by adopting Fourier infrared transform infrared spectrometer 2 The characterization is carried out, the scanning times are 32 times, and the resolution is 4cm -1 Wave number range 4000-400cm -1 。
Nano SiO 2 The infrared spectra of the particles before and after modification with 3-chloropropyltrimethoxysilane are shown in FIG. 2. 3446cm in the curve -1 And 1634cm -1 The nearby absorption peaks respectively correspond to the antisymmetric vibration and the bending vibration of water-OH; 1103cm -1 The absorption peak of (a) is antisymmetric stretching vibration of a Si-O-Si bond; 799cm -1 And 471cm -1 The absorption peaks in the vicinity correspond to the symmetric stretching vibration and bending vibration of the Si-O-Si bond, respectively. The modified nano silicon dioxide particles have methylene (-CH) in 3-chloropropyltrimethoxysilane at 2925cm-1 and 2853cm-1 2 -) and methyl (-CH) 3 ) The characteristic absorption peak shows that the 3-chloropropyltrimethoxysilane used for modification is covalently bonded with the surface of the nano-silica, so that the modifier is successfully covalently bonded to the surface of the nano-silica. It can be seen from curve 3 that the addition of hydrochloric acid solution advantageously enhances the modification effect.
(III) modifying the nano SiO 2 Preparing into aqueous solution, placing in a laser particle size analyzer, testing the particle size distribution as shown in figure 3, modifying with modified nanometer SiO 2 Has an average particle diameter Xav of 304.71nm. The particle size distribution of 400NTU of the Formazin standard solution is measured in a laser particle size analyzer as shown in FIG. 4, and the average particle size is Dav of 0.998 nm.
In the test process, the nano SiO before modification is found 2 The powder is easy to agglomerate in aqueous solution under the action of hydroxyl on the surface of silicon dioxide, the increase speed of the particle size change is high, and the stability is difficult to achieve; modified nano SiO 2 Due to the introduction of surface water-repellent groups, the nano SiO is reduced 2 The acting force of surface hydroxyl reduces the modified nano SiO 2 The agglomeration in the aqueous solution enhances the stability of the solution.
Placing the sample in an analytical instrument, and recording the particle size of the sample, the Formazin standard solution and the Formazin standard solution every five minutes in a standing stateNano SiO2 2 The particle diameter of the solution changes with time as shown in Table 1, and the change trend is shown in FIG. 5 (the change trend of the particle diameter of formalin in the Formazin standard solution) and FIG. 6 (the modified nanometer SiO 2 SiO in solution 2 Particle size trend graph). As can be seen from FIG. 3, the Formazin standard solution is agglomerated in a static state, the particle size of the Formazin standard solution is gradually increased, and in a test state, the particle size of the Formazin standard solution reaches a highest value after about 100 min and then is sharply reduced, because the Formazin standard solution is precipitated due to the agglomeration, and the particle size of the residual Formazin in water is small. Compared with the Formazin standard solution, the modified nano SiO 2 As the particle size thereof gradually becomes larger; siO with better particle size stability (FIG. 4), larger particle size due to gravity over time 2 The particles are slightly settled, the change rate of the particle size is 2.3 percent, and the modified nano SiO is seen 2 The solution has better stability.
TABLE 1 Formazin standard solution and modified nano SiO 2 Variation of particle size of solution with time
(IV) Linear relationship between modified silica solution concentration and turbidity: the turbidity of the water body is quantitatively characterized according to the scattering or attenuation degree of suspended particles in the water body to light rays without strict conversion relation between a scattering turbidity unit (NTU) and a mass concentration unit (mg/L). The variation of the scattered light is caused by the microscopically different shapes and particle size distributions of different suspended particles. Empirical formula is turbidity value (NTU) =0.13 × particulate matter concentration (mg/L). The invention corrects the empirical formula through experiments. Weighing modified silica with different qualities, and preparing aqueous solutions with different turbidity degrees by using three-stage water. Calibrating scatterometer with formalin standard solution to modify nanometer SiO 2 The concentration (mg/L) of the aqueous solution is used as the abscissa, the turbidity measurement value (NTU) is used as the ordinate, and a correlation curve is drawn, as shown in figure 7, so that the modified nano SiO is obtained 2 Concentration in aqueous solution (mg +)L) and turbidity (NTU) are as follows: y =0.1361x-2.2126, correlation coefficient R 2 Is 0.9995.
(V) modified silica solution dilution characteristics: to investigate the modified nano SiO 2 The dilution characteristic of the aqueous solution is to prepare the modified nano SiO with the turbidity of 813.7 NTU 2 And (3) diluting the solution in different proportions, and respectively testing the turbidity of the diluted solution by adopting a turbidity meter of the same model. Taking the calculated value of water solubility after dilution according to the proportion as the abscissa and the measured turbidity value (NTU) as the ordinate, and drawing a correlation curve, as shown in FIG. 8, to obtain the modified nano SiO 2 The aqueous solution dilution characteristic equation is as follows: y =1.01x +5.6076, correlation coefficient R 2 Is 0.9979. Thus, the modified nano SiO can be seen 2 The aqueous solution has good dilution characteristics.
(VI) Formazin solution and modified SiO 2 Study of standing stability of solution
Modification of nano SiO for comparison 2 Stability of the solution and the Formazin solution, and preparation of 412 NTU modified nano SiO 2 Solution (No. 1), in order to ensure the stability of the light source, it and 400NTU formalin standard solution (No. 2) were placed in a standard light source box, and their standing state at 0min, 30 min,60 min,90 min, 120 min,150 min,180 min was recorded, respectively, as shown in fig. 9.
After sufficient shaking, samples 1 and 2 were in homogeneous suspension as indicated by 0min. After standing for 30 min, the Formazin standard solution No. 2 showed clear layering on the upper end of the solution. The solution height of the clear part of solution No. 2 became larger and larger with the passage of time, and at 120 min, the bottom of the cuvette No. 2 appeared to be settled, and the flocs were clearly seen in the upper layer of solution. When the solution is placed for 180 min, the sediment is at the bottom of the clear solution which is the upper layer of the solution 2, and the uniformly dispersed suspension is still the solution 1. Therefore, the modified nano SiO 2 The standing stability of the solution is better than that of the Formazin solution.
Test 400NTU formalin standard solution and 412 NTU modified nanometer SiO separately 2 The turbidity of the solution varied with standing time as shown in Table 2。
TABLE 2 modified SiO 2 Turbidity change between solution and formalin standard solution
As can be seen from the data in Table 2 and FIG. 10, the turbidity of both solutions remained stable and unchanged in the first 20 min, the stability of both solutions was equivalent in the first 60min, and the turbidity of the Formazin standard solution was greatly reduced after 60min, which is identical to that shown in FIG. 9. The residual turbidity value of the Formazin standard solution is 47.8 percent and less than 50 percent when the Formazin standard solution is stood for 100 min, the turbidity value of the Formazin standard solution is only 25.5 percent of the initial state when the Formazin standard solution is stood for 120 min, and the modified SiO is 2 The haze value of the solution was 90.8% of the initial state, from which it was seen that modified SiO was present 2 The solution has better standing stability.
(VII) Formazin standard substance and modified SiO 2 Influence of the added standard substance on physical and chemical properties of water quality:
in the general water quality processor sanitary functional experiment, the labeling experiment of items such as oxygen consumption, turbidity, volatile, trichloromethane and the like can be synchronously carried out in the labeling experiment process of the filter element filtering component, so that the turbidity labeling substance is required not to influence indexes such as the pH value, the oxygen consumption, the volatile phenol, the trichloromethane and the like of water quality, and the configuration of the formalin labeling substance and the modified nano SiO 2 Volatile phenol, trichloromethane and other organic matters are not introduced in the preparation process, so that the pH value and the oxygen consumption are only used as the influence factors of the added standard substances on the water quality to be measured. Respectively testing tap water, formalin standard solution (25 NTU) and modified SiO 2 The pH and oxygen consumption of the spiked solution (25 NTU) are shown in Table 3:
TABLE 3 Formazin standards and modified SiO 2 Influence of the added standard substance on pH value and oxygen consumption of water
As can be seen from the data in Table 3, the modified SiO 2 The pH value and oxygen consumption of the standard liquid are not obviously changed, and the formalin can be oxidized by potassium permanganate to generate oxidation reaction, so that the oxygen consumption of the standard liquid is greatly changed. Formalin labeling liquid and modified SiO 2 The influence of the added standard solution on the pH value of water quality is not large. It can be seen that formalin labeling is not suitable for use as a labeling reagent in water quality processor labeling experiments.
Claims (7)
1. Modified nano SiO 2 The preparation method of the turbidity marking substance of the water quality processor is characterized in that the SiO is 2 Is spherical particle with average particle diameter of 100-500nm;
the method comprises the following steps:
(1) Weighing nano SiO 2 Dissolving in absolute ethyl alcohol, performing ultrasonic oscillation, and performing magnetic stirring to obtain silicon dioxide ethanol solution for later use;
(2) Adding 3-chloropropyltrimethoxysilane into the dispersed nano SiO 2 Performing constant-temperature water bath reaction in an ethanol solution, adding a proper amount of hydrochloric acid with the volume concentration of 3%, continuously reacting, continuously stirring in the reaction process, after the reaction is finished, performing centrifugal separation, washing for 3 times by using absolute ethyl alcohol, performing vacuum drying, and weighing a proper amount of modified nano SiO 2 Adding tertiary water into the powder, and ultrasonically dispersing the powder by 1h to prepare a standard solution;
the 3-chloropropyl trimethoxy silane and the nano SiO 2 The mass ratio of (A) is 2-3:1;
after a proper amount of 3% hydrochloric acid is added, the reaction is continued for 3.5h.
2. The method according to claim 1, wherein in the step (1), the nano SiO 2 The ratio of the absolute ethyl alcohol to the absolute ethyl alcohol is 1g:30mL.
3. The method according to claim 1 or 2, wherein in the step (1), the ultrasonic oscillation and the magnetic stirring are performed for 60min.
4. The preparation method according to claim 1, wherein the constant-temperature water bath reaction is carried out at 85 ℃ for 0.5h.
5. The method according to claim 1 or 4, wherein the hydrochloric acid is added in an amount of 1g nano SiO 2 1mL of the solution was added.
6. The method according to any one of claims 1 to 5, wherein the vacuum drying is oven drying at 55 ℃ for 8 hours.
7. Nano SiO prepared by the preparation method of any one of claims 1 to 6 2 The water quality processor turbidity adding standard substance is used.
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| AU2021102663A AU2021102663A4 (en) | 2020-10-30 | 2021-05-18 | Modified nano-sio2 spike material for turbidity of water treatment unit and preparation method thereof |
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