Production method of low-corrosion chlorine dioxide disinfectant

Abstract

The invention relates to the technical field of disinfectants, in particular to a production method of a low-corrosion chlorine dioxide disinfectant, which comprises the following steps: dropwise adding a sodium hydroxide solution, monitoring the pH value, adjusting the pH value to 8-10, maintaining stirring for 5 minutes, checking solubility and temperature, collecting precipitate particles, and filtering to remove the precipitate particles to obtain an alkaline mixed solution. According to the invention, the pH value is monitored and regulated to an alkaline interval to execute solubility inspection, so that the property control of the mixed solution is realized; on the basis of combined treatment of nanometer titanium dioxide photocatalysis and radio frequency discharge, the content of free radicals is multiplied, and the oxidation activity is improved; a silane coupling agent is combined to treat nano zirconium oxide and put into a system, the temperature is adjusted, the dispersion state is monitored, and the dispersion stability is guaranteed; the pH value and the oxidation-reduction potential are continuously monitored, foam separation and the chlorine content are controlled, and the quality of an intermediate solution is ensured; regulating and controlling the adding amount and the pH value of hydrochloric acid, monitoring gas escape, and screening out impurities to obtain a high-purity isolate.

Description

Technical Field

[0001] The present invention relates to the technical field of disinfectants, and in particular to a production method of a low-corrosion chlorine dioxide disinfectant. Background Art

[0002] The technical field of disinfectants is a professional field that studies and develops chemical agents for killing or inhibiting harmful microorganisms, mainly including aspects such as the formulation design, production process, quality control, usage methods, and safety assessment of various disinfectants. This field involves various types of disinfectants, such as chlorine-containing disinfectants, alcohol disinfectants, iodine disinfectants, quaternary ammonium salt disinfectants, etc. These disinfectants are widely used in fields such as medical and health, food processing, water treatment, and public place disinfection. In the existing production process, the monitoring means are single, it is difficult to timely grasp the reaction process status, resulting in low raw material utilization rate; there are blind spots in the quality control link, and a complete traceability chain has not been established, resulting in uneven product performance; and during the use process, due to the lack of targeted protection design, it is easy to cause corrosion to equipment and shorten the service life. Therefore, improvements are needed. Summary of the Invention

[0003] The purpose of the present invention is to solve the deficiencies existing in the prior art, and to propose a production method of a low-corrosion chlorine dioxide disinfectant.

[0004] To achieve the above purpose, the present invention adopts the following technical scheme. A production method of a low-corrosion chlorine dioxide disinfectant includes the following steps: Dropwise add a sodium hydroxide solution and monitor the pH value, adjust the pH value to the range of 8 to 10, maintain stirring for 5 minutes, check the solubility and temperature, collect the precipitate particles and filter them out to obtain an alkaline mixture; Based on the alkaline mixture, add nano-titanium dioxide and turn on ultraviolet light irradiation, control the light source intensity in the range of 350 to 400 nm, maintain the exposure for 10 minutes, apply radio frequency discharge and monitor the amount of free radicals generated to obtain an oxidation active solution; Based on the oxidation active solution, treat nano-zirconia with a silane coupling agent and add it to the system, adjust the temperature to 20 to 25 degrees Celsius, check the dispersion state of zirconium particles and mix them evenly, monitor the sedimentation rate and screen out the particles to obtain a protective dispersion; Based on the protective dispersion, monitor the pH value, adjust the range to 5 to 6, and at the same time measure the oxidation-reduction potential, maintain for 2 to 3 minutes, monitor the foam formation and separate the foam, record the chlorine content and compare the pH value change to obtain a chlorine dioxide intermediate solution; Based on the chlorine dioxide intermediate solution, add hydrochloric acid and monitor the gas evolution, adjust the pH value to 2 to 3 and maintain stirring for 3 minutes, collect the upper liquid phase and measure the temperature, record the turbidity and filter out the impurities to obtain a stable separation; Based on the stable isolate, detect the chloride ion concentration and record the value, adjust the concentration of the corrosion inhibitor added, maintain the temperature at 30 to 35 degrees Celsius and continuously stir for 10 minutes, detect the color change and complete the packaging to obtain the finished chlorine dioxide disinfectant.

[0005] Preferably, the steps for obtaining the alkaline mixture are specifically as follows: Based on the dropwise addition of the sodium hydroxide solution and monitoring of the pH value, conduct proportional weighing and slowly add the solution. At the same time, set the stirring speed to control the residence of suspended particles, and conduct observations on solubility and temperature. Finally, filter the precipitate and obtain a clear filtrate to get the precipitate filtrate; Based on the precipitate filtrate, re-monitor the pH value and calibrate the pH to the range of 8 to 10 with trace amounts of sodium hydroxide, monitor the change in solubility and adjust the stirring speed, and conduct impurity screening to obtain the pH-adjusted solution; Based on the pH-adjusted solution, separate the remaining suspended matter and use a filter screen to remove visible particles. At the same time, recheck the stability of the temperature and pH value, and collect the upper clear liquid to obtain the alkaline mixture.

[0006] Preferably, the steps for obtaining the oxidation active liquid are specifically as follows: Based on the alkaline mixture, add nano-titanium dioxide and ensure uniform distribution of the addition amount. At the same time, turn on the ultraviolet light and set the light source to the range of 350 to 400 nm, and conduct exposure records to obtain the initial light-exposed liquid; Based on the initial light-exposed liquid, continue the ultraviolet light exposure and apply radio frequency discharge. At the same time, use a detector to record the change in free radicals and compare the color of the solution, and pay attention to the solution temperature to obtain the active obtained liquid; Based on the active obtained liquid, interrupt the ultraviolet light exposure and turn off the radio frequency discharge, use a filter cloth to intercept suspended fine particles and separate the upper clear solution, and recheck the temperature and then collect the transparent liquid phase to obtain the oxidation active liquid.

[0007] Preferably, the steps for obtaining the protective dispersion are specifically as follows: Based on the oxidation active liquid, confirm the ratio of silane coupling agent and nano-zirconia and add zirconium particles to the solution, and stir to promote mixing to obtain a zirconium premix; Based on the zirconium premix, adjust the ambient temperature to 20 to 25 degrees Celsius and control the stirring speed, and continuously check the uniform dispersion of particles for 2 minutes to obtain a zirconium uniformly dispersed liquid; Based on the zirconium uniformly dispersed liquid, monitor the sedimentation rate and screen out particles, and detect the temperature of the upper liquid phase and the number of visible particles. Finally, collect the clear solution to obtain the protective dispersion.

[0008] Preferably, the steps for obtaining the chlorine dioxide intermediate solution are specifically as follows: Based on the protective dispersion liquid, the pH value is measured and adjusted to the range of 5 to 6 with an acid-base solution. Meanwhile, the redox potential value is examined and recorded to obtain a pH-regulated mixed solution. Based on the pH-regulated mixed solution, stirring is maintained for 2 to 3 minutes and the foam formation is monitored. Then, a separation device is used to remove the foam and retain the clear liquid, and the chlorine content measurement value is recorded to obtain a foam-separated liquid. Based on the foam-separated liquid, the recorded pH value is compared with the initial value to check the fluctuation range. Meanwhile, the solution temperature and redox potential are measured to obtain a stable and transparent liquid, thus obtaining an intermediate chlorine dioxide solution.

[0009] Preferably, the steps for obtaining the stable separated substance are specifically as follows: Based on the intermediate chlorine dioxide solution, hydrochloric acid is added dropwise in proportion and the gas evolution rate is monitored. Then, a stirring device is used to maintain for 1 minute to obtain an acidified mixed solution. Based on the acidified mixed solution, a pH meter is used to correct the pH to the range of 2 to 3 and continuous stirring is carried out for 2 minutes. The change in the number of bubbles and turbidity is detected, and the upper liquid phase is collected to obtain an acidified clarified solution. Based on the acidified clarified solution, re-filtration is carried out to remove residual solid substances, and the temperature and turbidity are recorded. After separating the clarified solution, it is loaded to obtain a stable separated substance.

[0010] Preferably, the steps for obtaining the finished chlorine dioxide disinfectant are specifically as follows: Based on the stable separated substance, the chloride ion concentration is detected and the value is recorded. Then, a corrosion inhibitor is weighed and prepared for dosing to obtain a pre-liquid of the corrosion inhibitor. Based on the pre-liquid of the corrosion inhibitor, the corrosion inhibitor is added and maintained at 30 to 35 °C. Meanwhile, continuous stirring is carried out for 5 minutes and the change in the chloride ion concentration is repeatedly recorded to obtain a corrosion inhibitor mixed solution. Based on the corrosion inhibitor mixed solution, stirring is extended for 5 minutes and the color change is observed. The transparent upper layer solution is separated and the final temperature is rechecked. After packaging, the finished product is obtained, thus obtaining the finished chlorine dioxide disinfectant.

[0011] Compared with the prior art, the advantages and positive effects of the present invention are as follows: The present invention performs solubility inspection by monitoring and regulating the pH value to an alkaline range to achieve the control of the properties of the mixed solution; based on the combined treatment of nano-titanium dioxide photocatalysis and radio frequency discharge, the content of free radicals is doubled and the oxidation activity is enhanced; by combining the treatment of nano-zirconia with silane coupling agent and adding it to the system, the temperature is adjusted and the dispersion state is monitored to ensure dispersion stability; continuously monitoring the pH value and redox potential, controlling foam separation and chlorine content to ensure the quality of the intermediate solution; regulating the dosage of hydrochloric acid and the pH value, monitoring gas evolution and screening impurities to obtain a highly pure separated substance; coordinating the adjustment of the concentration of the corrosion inhibitor and temperature control to form a product with both disinfection and low corrosion performance. Introducing the composite technology of photocatalysis and radio frequency discharge to promote the rapid generation of active ingredients; adopting the surface modification and dispersion technology of nano-materials to enhance the product stability. Brief Description of the Drawings

[0012] Figure 1 It is a schematic diagram of the steps of the present invention. Detailed Embodiment

[0013] In order to make the objectives, technical solutions and advantages of the present invention clearer and more understandable, the present invention will be further described in detail below with reference to the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0014] Please refer to Figure 1 , the present invention provides a technical solution, a production method of a low-corrosion chlorine dioxide disinfectant, including the following steps: Dropwise add sodium hydroxide solution and monitor the pH value, adjust the pH value to the range of 8 to 10, maintain stirring for 5 minutes, check the solubility and temperature, collect the precipitate particles and filter them off to obtain an alkaline mixed solution; Based on the alkaline mixed solution, add nano-titanium dioxide and turn on the ultraviolet light irradiation, control the light source intensity in the range of 350 to 400 nm, maintain the exposure for 10 minutes, apply radio frequency discharge and monitor the amount of free radicals generated to obtain an oxidation-active solution; Based on the oxidation-active solution, treat nano-zirconia with silane coupling agent and add it to the system, adjust the temperature to 20 to 25 degrees Celsius, check the dispersion state of zirconium particles and mix them evenly, monitor the sedimentation rate and screen out the particles to obtain a protective dispersion solution; Based on the protective dispersion solution, monitor the pH value, regulate the range to 5 to 6, simultaneously measure the redox potential, maintain for 2 to 3 minutes, monitor the foam formation and separate the foam, record the chlorine content and compare the pH value change to obtain a chlorine dioxide intermediate solution; Based on the chlorine dioxide intermediate solution, add hydrochloric acid and monitor the gas evolution, adjust the pH value to 2 to 3 and maintain stirring for 3 minutes, collect the upper liquid phase and measure the temperature, record the turbidity and filter off the impurities to obtain a stable separated substance; Based on the stable isolate, detect the chloride ion concentration and record the value, adjust the concentration of the corrosion inhibitor added, maintain the temperature at 30 to 35 degrees Celsius and continuously stir for 10 minutes, detect the color change and complete the packaging to obtain the finished chlorine dioxide disinfectant.

[0015] The steps for obtaining the alkaline mixture are specifically as follows: Based on the dropping of the sodium hydroxide solution and monitoring the pH value, conduct proportional weighing and slowly add the solution. At the same time, set the stirring speed to control the residence of suspended particles, and conduct solubility and temperature observations. Finally, filter the precipitate and obtain a clear filtrate to get the precipitate filtrate; Based on the precipitate filtrate, re-monitor the pH value and calibrate the pH to the range of 8 to 10 with trace amounts of sodium hydroxide, monitor the change in solubility and adjust the stirring speed, and conduct impurity screening to obtain the pH-adjusted solution; Based on the pH-adjusted solution, separate the remaining suspended matter and use a filter screen to remove visible particles. At the same time, recheck the stability of the temperature and pH values, and collect the upper clear liquid to obtain the alkaline mixture.

[0016] Specifically, based on the dropping of the sodium hydroxide solution and monitoring the pH value. During this process, first weigh the mass or volume of the sodium hydroxide solution according to the pre-set feeding ratio value, read the value of the current solution with a pH meter and compare the measured pH with the reference range. For example, recheck when the pH is below 2 or above 14. Keep the feeding speed stable when adding the sodium hydroxide solution and use a stirring device to maintain the state of suspended particles in the middle of the solution. If local deposition or uneven suspension of particles is observed, gradually fine-tune the stirring speed. Insert the temperature sensor into the solution and compare the measured temperature with the interval value set by experience. For example, use 20°C to 60°C as the effective range for dissolution and suspension monitoring. If the temperature exceeds this range, record it and prompt an abnormality to the operation control link. In the solubility test stage, the solute dissolution rate can be obtained according to a spectrophotometer or other detection means, and it is compared with the pre-determined reference dissolution rate table. If the dissolution rate data remains stagnant at a low level for a long time, readjust the feeding or repeat the stirring process. When the dissolution rate rises to a stable interval and the deviation between two consecutive readings is less than 1%, the dissolution process is considered close to completion. Then, select a filter screen or a vacuum filtration device to separate the insoluble matter and observe the transparency of the filtrate. Compare the number of impurity particles in the filtered solution with the highest particle number threshold set by experimental experience, such as 50 particles of impurities / 100 ml. If it exceeds this threshold, continue with the supplementary filtration operation. When the filtrate is basically clear, continue to maintain the operating environment temperature and observe again whether the pH meets the pre-set safety range. Finally, retain the clear filtrate to obtain the precipitate filtrate.

[0017] Based on the precipitation filtrate, when re - monitoring the pH value, first obtain the precipitation filtrate sample mentioned above and use a pH meter to check the value. If the value is less than 8, add a small amount of sodium hydroxide solution drop - by - drop to the solution and stir after each addition to make the alkaline components evenly distributed. At the same time, use a thermometer to detect the temperature of the solution before and after adding the material. If the temperature is outside the range of 20°C to 60°C, record the abnormality and then use external refrigeration or heating methods to bring the temperature back to this range. When the pH gradually approaches the range of 8 to 10, summarize and record each correction amount, and detect the change in solubility. Compare the current solubility with the solubility of the precipitation filtrate obtained previously. If the dissolution rate is detected to be stable and the comparison deviation is within 1%, it indicates that the solubility meets the standard. Then continue to stir and use a sieve to check whether there are impurity lumps or fibrous substances. If the detected impurity content exceeds the maximum visible impurity threshold specified in the experimental experience, such as 10 visible particles / 100 ml, then perform a low - speed sedimentation or higher - precision filtration again. If the impurity content does not exceed this threshold, stop the sieving operation and finally use a pH meter to confirm that the pH value is in the range of 8 to 10 to obtain the pH - adjusted solution.

[0018] Based on the pH - adjusted solution, when separating the remaining suspended solids, first check with the naked eye and an optical detector whether the suspended solids are lower than the maximum observable particle concentration threshold established by experience in advance, such as 10 impurities / 100 ml. If it is observed that the particles significantly exceed this threshold, use a filter screen or centrifugation for additional separation and then perform pH value and temperature detection again. Compare the current pH value with the range of 8 to 10 recorded previously. If the deviation exceeds 0.5, continue to finely adjust the sodium hydroxide dosage and keep stirring. After verifying that the pH value is stable, perform a temperature review, comparing the measured temperature value with the normal range of 20°C to 60°C. If the temperature is higher than 60°C or lower than 20°C, record the abnormality and perform corresponding heating or cooling treatment. After all the excess suspended solids and visible particles are removed through multiple cycle detections, when collecting the clarified liquid from the upper layer of the container, first observe the color and transparency of the solution and compare with the normal transparency standard mentioned above. If the color is turbid, there may be fine particles and it needs to be filtered again. When the light transmittance of the solution reaches the established empirical standard under visible light, such as the light transmittance is greater than 90%, the separation process can be ended, and the final clarified liquid is retained to obtain the alkaline mixture.

[0019] The specific steps for obtaining the oxidation - active liquid are as follows: Based on the alkaline mixture, add nano - titanium dioxide and ensure that the dosage is evenly distributed. At the same time, turn on the ultraviolet light and set the light source to the range of 350 to 400 nm, and record the exposure to obtain the initial light - irradiated liquid. Based on the initial light - irradiated liquid, continue the ultraviolet light irradiation and apply radio - frequency discharge. At the same time, use a detector to record the change in free radicals and compare the solution color, and pay attention to the solution temperature to obtain the active - obtained liquid. Based on the active obtained liquid, interrupt the ultraviolet light irradiation and turn off the radio frequency discharge. Use a filter cloth to intercept suspended fine particles and separate the upper clarified solution. After temperature verification, collect the transparent liquid phase to obtain the oxidation active liquid.

[0020] Specifically, based on the alkaline mixture, when adding titanium dioxide nanoparticles, weigh the titanium dioxide nanoparticles according to the preset addition ratio in advance. During the addition process, divide the solid particles into several portions and add them to the solution in batches. Immediately stir after each addition to make the solid disperse more evenly. Then, cooperate with ultraviolet light irradiation and set the light source wavelength range to 350 nm to 400 nm. At the same time, record the exposure duration of the ultraviolet light irradiation in seconds. Check whether the cumulative exposure requirement is met by comparing with the reference value of the optimal light exposure duration set based on previous experience, such as 60 seconds to 300 seconds. After the addition is completed, continue to observe the suspension state of the titanium dioxide nanoparticles in the solution. If obvious agglomeration phenomena are found and the diameter of the agglomerated particles exceeds the designed threshold, such as 5 μm, interrupt the light irradiation and adjust the stirring intensity. After confirming that the particles are well dispersed, restart the ultraviolet light source and record the total exposure duration. Finally, compare the solution after the exposure is completed with the camera imaging data to confirm the actual light irradiation effect. When the record shows that the established exposure duration has been reached, mark this solution as the initial light irradiation liquid.

[0021] Based on the initial light irradiation liquid, when continuing the ultraviolet light irradiation and applying radio frequency discharge, first place the initial light irradiation liquid in a container with a radio frequency electrode. Set the radio frequency power value to be between 20 W and 50 W for reference. Check the power output through a radio frequency power meter. If it is lower than 20 W, it means that the discharge is insufficient and the set value needs to be adjusted. If it exceeds 50 W, it indicates that there may be excessive energy causing the solution to heat up too fast and conduct an inspection. During the discharge process, use a detector to track the change of free radicals. Compare the current free radical level through methods such as chemiluminescence or conductivity. Conduct a difference statistics on the free radical values obtained from the real-time detection and the basic values of the previous step of the initial light irradiation liquid before the radio frequency discharge. If the increase is less than 5%, increase the discharge duration. If the increase exceeds 30%, reduce the discharge power or shorten the discharge time. At the same time, compare the color of the solution through visible light detection. Check the color against the reading of the reference color card or colorimeter. If there is a significant deviation in the color, record it again and check whether there is an abnormal reaction. Keep the solution temperature monitored within the range of 20°C to 60°C. When the discharge reaches the target increase in free radicals listed in the operation process, stop the radio frequency discharge. Finally, obtain the active obtained liquid.

[0022] Based on the active liquid obtained, after interrupting the ultraviolet light irradiation and turning off the radio frequency discharge, first place a filter cloth on the experimental bench, slowly pour out the liquid to intercept the suspended fine particles in the solution, and compare the solid particles collected on the filter cloth with a preset acceptable particle number threshold, such as 10 impurities / 100 ml. If it exceeds this threshold, it may be necessary to recheck the previous light irradiation and discharge steps or perform secondary filtration here. If it does not exceed, continue to retain the filtered clear solution. Use a thermometer to recheck the temperature of this clear solution and compare it with the previously recorded temperature requirement. If the temperature deviates from 20°C to 60°C, perform heating or cooling operations. After confirming that the value enters the normal range, conduct a light transmittance detection again to check whether there are still fine particles remaining. When the light transmittance is greater than 90%, collect this transparent liquid phase and mark the relevant detection values to obtain the oxidation active liquid.

[0023] The steps for obtaining the protective dispersion are specifically as follows: Based on the oxidation active liquid, confirm the ratio of the silane coupling agent and nano-zirconia, add the zirconium particles to the solution, and stir to promote mixing to obtain a zirconium premixed liquid; Based on the zirconium premixed liquid, adjust the ambient temperature to 20 to 25 degrees Celsius, control the stirring speed, and continuously check the particle dispersion uniformity for 2 minutes to obtain a zirconium uniformly dispersed liquid; Based on the zirconium uniformly dispersed liquid, monitor the sedimentation rate, screen out the particles, detect the temperature of the upper liquid phase and the number of visible particles, and finally collect the clear solution to obtain the protective dispersion.

[0024] Specifically, based on the oxidation active liquid obtained previously and referring to the summarized ratio entries of silane coupling agent and nano-zirconia, first confirm the specific mass ratio and then add zirconium particles step by step. Before adding, the solid content and free radical concentration in the previously obtained oxidation active liquid can be compared. For example, compare the free radical concentration with the reference range. If the detected value is between 5 mg / L and 15 mg / L, it meets the initial requirements. If it is lower than 5 mg / L, supplementary exposure is carried out. If it exceeds 15 mg / L, short-term static settlement is carried out to observe the color stability. Subsequently, weigh the silane coupling agent and nano-zirconia according to the registered ratio entries. Here, the ratio data is usually obtained from multiple experiments or statistical experience of the same type of process. For example, premix and screen the coupling agent and zirconium particles at a mass ratio of 5:1 or 10:1. When it is confirmed that a certain ratio conforms to the on-site detection data and there is no significant difference, slowly add the corresponding zirconium particles into the solution and continuously stir. When stirring, monitor the rotation speed through a tachometer and select a suitable rotation speed within the range of 200 rpm to 400 rpm. If a large number of agglomerated particles are found, the rotation speed can be moderately adjusted or the zirconium particles can be dispersed first. When the suspension is relatively uniform, use a thermometer to detect the solution temperature and compare it with the previously set range of 20°C to 40°C. If the temperature exceeds this range, cooling or heating treatment is carried out. When stirring for about two minutes, observe the overall stability of the particle suspension in the solution. If there is obvious sedimentation or floating, the addition comparison and stirring process are carried out again. Finally, a zirconium premixed liquid is obtained.

[0025] Based on the zirconium premixed liquid, when adjusting the ambient temperature to 20°C to 25°C, first use temperature control equipment to observe the indoor and solution temperatures, and then compare the actual detected value with this range. If the temperature is higher than 25°C, cooling treatment is applied. If it is lower than 20°C, heating compensation is carried out. After the temperature is stable, set the stirring speed. For example, use a tachometer to maintain it at the middle section of 200 rpm to 400 rpm. If large-scale stratification of particles occurs, increase the stirring intensity. If the particles rotate at high speed and collide frequently, reduce the rotation speed. When it is observed that there is no obvious segregation or local accumulation of particles in the solution, start timing for about 2 minutes, record the distribution image of the particles in the solution every 30 seconds, and compare the particle concentration in the image with the experience comparison table. For example, check whether the number of obvious aggregation areas in a single-frame image exceeds 1. If it exceeds, it means the dispersion is uneven and the stirring needs to be finely adjusted. When recording again until the particle distribution is basically the same as the dispersed state in the reference diagram, it is considered that the uniformity meets the standard. Finally, a zirconium uniformly dispersed liquid is obtained.

[0026] Based on the zirconium uniform dispersion liquid, when monitoring the sedimentation rate, first keep the solution static and observe the sedimentation of particles at fixed time intervals. Record the change in the interface position between the clear liquid and the turbid liquid every 30 seconds using a graduated measuring cylinder. Then, compare it with the specifications of the nano-zirconia particles and the previously measured liquid viscosity parameters. If the sedimentation interface shows a significant downward shift within 60 seconds and the downward shift height exceeds the set threshold, such as 5 mm, it indicates that the particles sediment quickly, and it may be considered to adjust the viscosity or dispersion ratio. If the sedimentation rate is overall slow and there is no significant fluctuation in the interval from 30 seconds to 60 seconds, proceed to the next step of sieving. The sieving process can be carried out by visual or optical detection methods. Filter out when the monitored particle size exceeds 5 μm or there are too many aggregates. If the number of visible particles remains below the empirical value of less than 10 visible particles / 100 ml, end the sieving. Subsequently, measure the temperature of the upper liquid phase and compare it with the range of 20°C to 25°C. If the value is within this range, continue to collect the clarified solution, and finally obtain the protective dispersion liquid.

[0027] The steps for obtaining the chlorine dioxide intermediate solution are specifically as follows: Based on the protective dispersion liquid, measure the pH value and adjust it to the range of 5 to 6 with acid-base solutions. At the same time, check and record the redox potential value to obtain the pH-regulated mixed solution; Based on the pH-regulated mixed solution, keep stirring for 2 to 3 minutes and monitor the foam formation. Use a separation device to remove the foam and retain the clear liquid, and record the chlorine content measurement value to obtain the foam-separated liquid; Based on the foam-separated liquid, compare the recorded pH value with the initial value and check the fluctuation range. At the same time, measure the solution temperature and redox potential to obtain a stable and transparent liquid, and obtain the chlorine dioxide intermediate solution.

[0028] Specifically, based on the protective dispersion liquid, when measuring the pH value, first use a pH meter to detect the current solution value. Compare the measured reading with the range of 5 to 6. If the detected value is less than 5, add alkaline solution in batches for adjustment. If the detected value is greater than 6, add acidic solution for step-by-step correction. Observe the solution color after each addition and use the pH meter for verification again. Compare the value read by the redox potential detector with the registered control data. If the potential value deviates from the reference range, such as 200 mV to 400 mV, stir briefly after recording to allow the solution to re-equilibrate. The dosage of the additive is determined according to the change in pH each time. For example, if the pH only changes by about 0.1 after one adjustment, appropriately increase the addition rate. If the change exceeds 1 after one adjustment, reduce the addition speed and measure the solution temperature again. When the pH remains within the range of 5 to 6 for two consecutive times and the redox potential is stable, obtain the pH-regulated mixed solution.

[0029] Based on the pH-regulated mixture, during the 2 - 3 minutes of continuous stirring, observe the foam generation status at regular intervals. Record the height of the foam layer every 30 seconds and compare it with the safety threshold specified in the experimental experience, such as a height of 2 cm. If the foam height exceeds this threshold, check whether defoamer needs to be added after recording the data. If the foam height rapidly decreases within a short period, continue to maintain the stirring. After the detected foam tends to be stable, use a separation device to remove the foam part and retain the clear liquid. Then, measure the chlorine content using titration or ion-selective electrode method. If there is a large deviation between the chlorine concentration and the previously referenced target value, continue to confirm whether the pH needs to be corrected again or the stirring time needs to be extended. When the chlorine content gradually approaches the target set range and no significant drift occurs, finally obtain the foam separation liquid.

[0030] Based on the foam separation liquid, when comparing the recorded pH value with the initial value, first call the previously obtained pH detection results and the current readings for differential statistics. If the pH value fluctuates by no more than 0.2, it indicates a stable state. If the fluctuation is greater than 0.2, add a small amount of regulating liquid for fine-tuning after recording the data. At the same time, measure the current solution temperature and compare it with the range of 20°C to 25°C. If the temperature deviates from this range, perform short-term heating or cooling. After confirming that the temperature has returned to the specified range, conduct the redox potential detection. If the potential value differs from the previously read data by more than 50 mV, increase the detection frequency and compare the chlorine content until the results of multiple measurements are close to the reference value and the fluctuations are small. After integrating these values, it indicates that the solution is in a relatively transparent and stable state, and finally obtain the chlorine dioxide intermediate solution.

[0031] The steps for obtaining the stable separation are as follows: Based on the chlorine dioxide intermediate solution, add hydrochloric acid dropwise in proportion and monitor the gas evolution rate, and use a stirring device to maintain for 1 minute to obtain an acidified mixture; Based on the acidified mixture, use a pH meter to adjust the pH to the range of 2 - 3 and continuously stir for 2 minutes, and detect the change in the number of bubbles and turbidity, and collect the upper liquid phase to obtain an acidified clarified liquid; Based on the acidified clarified liquid, perform filtration again to remove residual solid substances and record the temperature and turbidity. After separating the clarified solution, load it to obtain the stable separation.

[0032] Specifically, based on the chlorine dioxide intermediate solution obtained above and referring to the sorted hydrochloric acid ratio parameters, first select the hydrochloric acid concentration range of, for example, 30% to 35% as the basis for dropping. Slowly add it to the solution at a rate of 5 mL to 10 mL each time and simultaneously observe the reading of the gas flowmeter. If the reading exceeds the empirical threshold of 20 mL per minute, stop dropping and record the gas discharge time. During the pause, monitor the solution temperature with a thermometer and compare it with the reference range of 20°C to 40°C. If the temperature is lower than 20°C, use heating to increase the temperature. If the temperature is higher than 40°C, use cooling measures to bring it back to the normal range. At the same time, set the rotation speed of the stirring device at 200 rpm to 300 rpm and record the bubble morphology on the surface of the solution after stirring every 30 seconds. When the bubble increment gradually stabilizes and the gas flow fluctuates between 10 mL and 15 mL per minute during two consecutive detections, continue to add hydrochloric acid in batches incrementally and compare with the above threshold again to confirm no significant abnormality. Finally, after the addition is completed, keep stirring for about 1 minute and check the appearance change and temperature stability of the solution. If the bubbles are basically stable and the temperature deviation does not exceed 1°C, stop dropping to obtain the acidified mixture.

[0033] Based on the acidified mixture and combined with the pH adjustment value range determined above, first use a pH meter to detect the current solution. If the detection result is less than 2, add a small dose of alkaline solution gradually. Measure the pH value again every 30 seconds after each addition and compare it with the reference range of 2 to 3. If the detection result is greater than 3, add a small amount of acidic solution for fine-tuning, and record the turbidity of the solution synchronously during each adjustment. Check whether particle aggregation occurs by visual inspection or an optical turbidity meter. If the turbidity is higher than the empirical threshold, for example, 20 NTU, conduct additional short-term sedimentation or rapid filtration under stirring conditions. When the turbidity is less than 10 NTU and the pH remains between 2 and 3, continue to stir for about 2 minutes and observe the number of bubbles every 30 seconds. If a large number of bubbles appear and form a foam layer with a height exceeding 2 cm, control the stirring speed or add a small amount of defoaming agent and observe again. After confirming that the bubbles gradually decrease and the pH and turbidity remain relatively stable, collect the upper liquid phase to obtain the acidified clarified liquid.

[0034] Based on the acidified clarified liquid and in accordance with the filter media selection criteria summarized in the filtration process list, first conduct rough filtration through filter paper or filter membrane with a filtration membrane pore size in the range of 5 μm to 10 μm. If it is detected that the residual solid particles after rough filtration are still more than the empirical threshold of 5 particles per 100 ml of solution, upgrade to multi-stage filter paper with a fine pore size, such as 1 μm to 3 μm, for re-filtration. During the filtration process, use a thermometer to detect the solution temperature. If the temperature deviates from the comparison range of 20°C to 40°C, adjust the solution by heating or cooling, and observe the turbidity meter reading. If it has dropped below 10 NTU, it indicates that most of the impurity particles have been intercepted. After recording the temperature and turbidity at this moment, further separate and load the filtered clarified solution into a designated container to finally obtain a stable separation.

[0035] The steps to obtain the finished chlorine dioxide disinfectant are specifically as follows: Based on the stable separation, conduct a chloride ion concentration detection and record the value, and weigh the corrosion inhibitor for preparation of the dosing to obtain the pre-liquid of the corrosion inhibitor; Based on the pre-liquid of the corrosion inhibitor, add the corrosion inhibitor and maintain at 30 to 35 degrees Celsius, while continuously stirring for 5 minutes and repeatedly record the change in chloride ion concentration to obtain the corrosion inhibitor mixture; Based on the corrosion inhibitor mixture, extend the stirring for 5 minutes and observe the color change, separate the transparent upper layer solution and recheck the final temperature, and obtain the finished product after packaging to obtain the finished chlorine dioxide disinfectant.

[0036] Specifically, based on the stable separation and according to the chloride ion concentration detection method listed above, first obtain a solution sample and then use an ion-selective electrode or titration method to determine the chloride ion content. If the value is lower than 50 mg / L, after recording this result, confirm the compatibility of this concentration with the subsequent dosing of the corrosion inhibitor. If the value is higher than 200 mg / L, after re-detecting to exclude reading errors, prompt that additional dilution of the solution may be required. Register the final chloride ion value and weigh the corrosion inhibitor. For example, weigh the inhibitor according to a certain mass ratio or volume ratio. After weighing, confirm the compatibility of this inhibitor with the previously registered chloride ion concentration in combination with the on-site process comparison table to obtain the pre-liquid of the corrosion inhibitor.

[0037] Based on the pre-liquid of the corrosion inhibitor and according to the previously weighed inhibitor dosing plan, add while observing the color change of the solution within the range of 30°C to 35°C. If the color is too dark, the dosing speed can be slowed down or supplemented in portions to maintain overall stability. After dosing, set the stirring speed at 200 rpm to 300 rpm and continue for 5 minutes. Use an ion-selective electrode to repeatedly read the chloride ion concentration every 1 minute. If the monitoring value fluctuates by more than 10%, re-compare the dosing amount. When the concentration change is maintained within 5% and there is no obvious turbidity in the appearance of the solution, continue to confirm that the temperature does not deviate from the range of 30°C to 35°C, and finally obtain the corrosion inhibitor mixture.

[0038] Based on the corrosion inhibitor mixture, maintain stirring for another 5 minutes, and then compare the solution color every 1 minute. If there is an obvious lightening or darkening, compare it with the empirical threshold. For example, according to the colorimetric card, if the established deviation range is met, stirring can continue. If the color deviates from the preset standard for a long time, after recording the value, add a small amount of inhibitor or adjust the stirring speed and observe again. Stop stirring when the color gradually returns to the target reference color and the chloride ion detection value no longer fluctuates violently. Then let the solution stand still and wait for the upper transparent area to separate. Slowly take out the transparent solution and check that its final temperature is still between 30°C and 35°C. Package the solution and note the relevant detection parameters on the label to obtain the finished chlorine dioxide disinfectant.

[0039] The above are only the preferred embodiments of the present invention, and do not limit the present invention in other forms. Any person skilled in the art may use the technical content disclosed above to make changes or modifications into equivalent embodiments with equivalent changes and apply them to other fields. However, as long as it does not depart from the technical solution content of the present invention, any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention still fall within the protection scope of the technical solution of the present invention.

Claims

1. A method for producing a low-corrosive chlorine dioxide disinfectant, characterized in that: The following steps are involved: Add sodium hydroxide solution dropwise and monitor the pH value, adjust the pH value to the range of 8 to 10, maintain stirring for 5 minutes, check the solubility and temperature, collect the precipitated particles and remove them by filtration to obtain an alkaline mixed solution; Based on the alkaline mixed solution, nano titanium dioxide is added and ultraviolet light irradiation is turned on, the light source intensity is controlled within the range of 350 to 400 nm, the exposure is maintained for 10 minutes, radio frequency discharge is applied and the amount of free radical generation is monitored to obtain an oxidizing active liquid; Based on the oxidizing active liquid, nano zirconium oxide is treated with a silane coupling agent and added into the system, the temperature is adjusted to 20 to 25 degrees Celsius, the dispersion state of zirconium particles is checked and mixed, the sedimentation rate is monitored and particles are screened out to obtain a protective dispersion; Based on the protective dispersion, pH value monitoring is performed, the range is adjusted to 5 to 6, and the redox potential is measured at the same time, and the redox potential is maintained for 2 to 3 minutes, the foam is monitored and separated, the chlorine content is recorded and the pH value change is compared to obtain a chlorine dioxide intermediate solution; Based on the chlorine dioxide intermediate solution, hydrochloric acid is added and gas evolution is monitored, the pH value is adjusted to 2 to 3 and stirring is maintained for 3 minutes, the upper liquid phase is collected and the temperature is measured, the turbidity is recorded and impurities are removed by filtration to obtain a stable separation; Based on the stable isolate, the chloride ion concentration is detected and the value is recorded, the concentration of the added corrosion inhibitor is adjusted, the temperature is maintained at 30 to 35 degrees Celsius and stirred continuously for 10 minutes, the color change is detected and the packaging is completed to obtain a finished chlorine dioxide disinfectant.

2. The method for producing a low-corrosive chlorine dioxide disinfectant according to claim 1, characterized in that: The steps of obtaining the alkaline mixed solution are specifically as follows: Based on the dripping of sodium hydroxide solution and monitoring of pH value, proportional weighing is performed and the solution is slowly added, while the stirring speed is set to control the retention of suspended particles, and the solubility and temperature are observed, and finally the precipitate is filtered to obtain a clear filtrate to obtain a precipitate filtrate; Based on the precipitation filtrate, the pH value is monitored again and the pH is corrected to the range of 8 to 10 with a trace amount of sodium hydroxide, the solubility change is monitored and the stirring speed is adjusted, and impurities are screened to obtain a pH adjusted solution; Based on the pH adjusting liquid, the remaining suspended matter is separated and visible particles are removed using a filter, while the temperature and pH value stability are reviewed, and the upper clear liquid is collected to obtain an alkaline mixed liquid.

3. The production method of the low-corrosion chlorine dioxide disinfectant according to claim 1, characterized in that: The steps of obtaining the oxidation active liquid are specifically as follows: Based on the alkaline mixed solution, nano titanium dioxide is added and the amount of the added is ensured to be evenly distributed, while ultraviolet light is turned on and the light source is set to a range of 350 to 400 nm, and exposure records are performed to obtain an initial light-irradiated solution; Based on the initial solution irradiated with light, ultraviolet light is continued and radio frequency discharge is applied, while a detector is used to record the change of free radicals and compare the solution color, and the solution temperature is paid attention to, so as to obtain an active solution; Based on the activity, a liquid is obtained, the ultraviolet irradiation is interrupted and the radio frequency discharge is turned off, a filter cloth is used to intercept the suspended fine particles and separate the upper clear solution, and the transparent liquid phase is collected after temperature verification to obtain an oxidative active liquid.

4. The method for producing a low-corrosive chlorine dioxide disinfectant according to claim 1, characterized in that: The steps of obtaining the protective dispersion are specifically as follows: Based on the oxidizing active liquid, confirm the ratio of silane coupling agent and nano zirconium oxide, add zirconium particles into the solution, and stir to promote mixing to obtain a zirconium premixed solution; Based on the zirconium premix, the ambient temperature is adjusted to 20 to 25 degrees Celsius and the stirring speed is controlled, and the particle dispersion uniformity is checked for 2 minutes to obtain a uniform zirconium dispersion; Based on the uniform zirconium dispersion, the sedimentation rate is monitored and particles are screened out, and the upper liquid phase temperature and the number of visible particles are detected. Finally, the clarified solution is collected to obtain the protective dispersion.

5. The method for producing a low-corrosive chlorine dioxide disinfectant according to claim 1, characterized in that: The steps for obtaining the chlorine dioxide intermediate solution are specifically as follows: Based on the protective dispersion, the pH value is measured and adjusted to a range of 5 to 6 with an acid-base solution, and the redox potential value is checked and registered to obtain a pH-controlled mixed solution; Based on the pH-controlled mixed solution, stirring is maintained for 2 to 3 minutes and the foam is monitored, and a separation device is used to remove the foam and retain the clear liquid, and the chlorine content measurement value is recorded to obtain a foam separation liquid; Based on the foam separation liquid, the recorded pH value is compared with the initial value and the fluctuation range is checked, and the solution temperature and redox potential are measured at the same time to obtain a stable transparent liquid and a chlorine dioxide intermediate solution.

6. The method for producing a low-corrosive chlorine dioxide disinfectant according to claim 1, characterized in that: The steps for obtaining the stable isolate are specifically as follows: Based on the chlorine dioxide intermediate solution, hydrochloric acid is added dropwise in proportion and the gas evolution rate is monitored, and a stirring device is used to maintain for 1 minute to obtain an acidified mixed solution; Based on the acidified mixed solution, a pH meter is used to calibrate the pH to a range of 2 to 3 and the mixture is continuously stirred for 2 minutes, and the number of bubbles and turbidity changes are detected, and the upper liquid phase is collected to obtain an acidified clarified solution; Based on the acidified clarified liquid, filtration was performed again to remove the residual solid matter and the temperature and turbidity were recorded. The clarified solution was separated and loaded to obtain a stable isolate.

7. The method for producing a low-corrosive chlorine dioxide disinfectant according to claim 1, characterized in that: The steps for obtaining the finished chlorine dioxide disinfectant are specifically as follows: Based on the stable separation, the chloride ion concentration is detected and the value is recorded, and the corrosion inhibitor is weighed to prepare for addition to obtain a corrosion inhibitor pre-liquid; Based on the corrosion inhibitor pre-liquid, adding corrosion inhibitor and maintaining at 30 to 35 degrees Celsius, while continuously stirring for 5 minutes and repeatedly recording the change of chloride ion concentration to obtain a corrosion inhibitor mixed solution; Based on the corrosion inhibitor mixture, stirring is extended for 5 minutes and the color change is observed, the transparent upper solution is separated and the final temperature is verified, and the finished product is obtained after packaging, thereby obtaining a finished chlorine dioxide disinfectant.

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