CN115363022A - Chlorine dioxide saturation slow-release technology with super-long-acting performance - Google Patents
Chlorine dioxide saturation slow-release technology with super-long-acting performance Download PDFInfo
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- CN115363022A CN115363022A CN202210080297.1A CN202210080297A CN115363022A CN 115363022 A CN115363022 A CN 115363022A CN 202210080297 A CN202210080297 A CN 202210080297A CN 115363022 A CN115363022 A CN 115363022A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/18—Vapour or smoke emitting compositions with delayed or sustained release
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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Abstract
The invention discloses a chlorine dioxide saturated slow release technology with super long-term efficiency.A saturated acid solution is prepared at first, a powdery molecular sieve is soaked in the saturated acid solution, then solid-liquid separation is carried out, the molecular sieve is roasted, and the processes are repeated for three times to achieve the aim of improving the content of acidic substances, so that a modified molecular sieve is obtained; coating and drying the sodium chlorite powder to obtain coated sodium chlorite; mixing the modified molecular sieve, the coated sodium chlorite, the sodium carboxymethylcellulose and the water-absorbent resin to obtain the chlorine dioxide long-acting slow-release agent; after the powder is hermetically packaged, the powder can be stored for a long time, and the storage period can reach more than 2 years; the long-acting slow release agent is mixed with purified water according to a proportion to be activated and begin to release chlorine dioxide gas; through the technology, the purification effect of the product can be greatly improved, the use cost of a user is greatly reduced, and the technology has great commercial value.
Description
Technical Field
The invention relates to the technical field of sterilization disinfectants and air purification, in particular to an ultra-long-acting chlorine dioxide saturated slow-release technology.
Background
Chlorine dioxide, as a grade A1 disinfectant confirmed by the world health organization, has been widely used for sterilization and disinfection in industries such as food, drinking water, medical health and the like, and in recent years, has also been widely used in the fields of air purification, food preservation, soil remediation and the like, and the chlorine dioxide sustained release agent (sustained release gel) has an especially prominent effect in the fields of air purification, food preservation and the like. However, chlorine dioxide gas is very active and volatile, so that it is difficult to store it for a long period of time, and chlorine dioxide gas has a certain risk and may explode when reaching a certain concentration.
The existing chlorine dioxide slow-release products are basically prepared by preparing chlorine dioxide gas by a chemical method, dissolving the chlorine dioxide gas in water to prepare chlorine dioxide aqueous solution, and then immobilizing chlorine dioxide by using a gel material to obtain the chlorine dioxide slow-release gel product. Because chlorine dioxide is generated in one step and the chlorine dioxide solution is volatilized rapidly, usually completely within 24 hours, the effective period of the product is completely determined by the slow release performance of the gel material. At present, the sustained-release period of most of gel substances is about 10 to 30 days, which causes great obstacles on the use effect and commercial promotion.
Disclosure of Invention
In view of the above-mentioned drawbacks and deficiencies of the prior art, it would be desirable to provide a saturated slow release technique for chlorine dioxide with ultra-long duration.
The invention provides a chlorine dioxide saturated slow release technology with super long-term efficiency, which comprises the following steps:
1) Preparing a saturated acid solution, and adding a powder molecular sieve into the saturated acid solution for soaking, wherein the soaking time is 24 hours, and the weight ratio of the powder molecular sieve to the saturated acid solution is 1-1;
2) Carrying out solid-liquid separation on the soaked molecular sieve, and roasting the molecular sieve after the solid-liquid separation at the roasting temperature of 200-800 ℃ for 2-5 h to obtain the modified molecular sieve;
3) Repeating the steps 1) and 2) for three times, wherein the two steps are used for storing acidic substances in the molecular sieve to the maximum extent by utilizing the adsorbability of the molecular sieve;
4) Coating and drying sodium chlorite powder, wherein the content of sodium chlorite in the sodium chlorite powder is more than or equal to 85 percent, and the granularity range of the sodium chlorite is 50-100 meshes; the coating material is one of sodium alginate and povidone; according to the weight ratio of the sodium chlorite powder to the sodium alginate of 5:1, drying the sodium chlorite powder and povidone according to a weight ratio of 5;
5) The modified molecular sieve, the coated sodium chlorite, the sodium carboxymethylcellulose and the water-absorbing resin are mixed according to the weight ratio of 17:4:3:1, mixing and processing to obtain powder A;
6) Adding purified water into the powder A, wherein the weight ratio of the purified water to the powder A is 1.
Preferably, the saturated acid solution is: including but not limited to one or more of hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, and citric acid.
Preferably, the roasting temperature and time are controlled, and the powder molecular sieve is 300-600 meshes.
Preferably, the molecular sieve is used to adsorb acidic substances to the maximum extent.
Preferably, the content of sodium chlorite in the sodium chlorite powder is more than or equal to 85 percent, and the granularity of the sodium chlorite ranges from 50 meshes to 100 meshes; the weight ratio of the sodium chlorite powder to the sodium alginate is 5:1, drying the sodium chlorite powder and povidone according to a weight ratio of 5-10 to obtain coated sodium chlorite, wherein the drying temperature is 80-120 ℃;
preferably, the modified molecular sieve, the coated sodium chlorite, the sodium carboxymethyl cellulose and the water-absorbing resin are mixed according to the weight ratio of 17:4:3:1, mixing for no less than 30 minutes;
preferably, the weight ratio of the purified water to the powder A is 1.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the ultra-long-acting binary chlorine dioxide sustained release agent, chlorine dioxide is not generated once, but acid substances are gradually dissolved into water to react along with volatilization, so that the reaction gradually proceeds along with volatilization, and the sustained release time is prolonged; a large amount of undissolved acid substances are remained on the modified molecular sieve, and along with the volatilization of the chlorine dioxide in the water, the acid substances are gradually dissolved into the solution to continue to react with the rest sodium chlorite, so that the generation amount of the chlorine dioxide is greatly increased. Thereby achieving the effect of non-one-time generation of chlorine dioxide in the sustained release agent, greatly improving the sustained release period, realizing the ultra-long release capacity of 6-12 months, and compared with the prior art, the sustained release period is improved by 6-12 times, so that the product effect and the commercial promotion aspect are greatly improved.
It should be understood that the statements made in this summary are not intended to limit the key or critical features of the embodiments of the present invention, or to limit the scope of the invention. Other features of the present invention will become apparent from the following description.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments made with reference to the following drawings:
FIG. 1 is a schematic diagram of the principle of saturated sustained release technology;
FIG. 2 is a chlorine dioxide content scale;
FIG. 3 is a table for recording the bactericidal effect of the slow-release type immobilized chlorine dioxide particles;
FIG. 4 is a table comparing degradation performance for formaldehyde;
FIG. 5 is a table of records of chlorine dioxide slow release period measurements (chlorine dioxide release rate > 180. Mu.g/h).
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
Referring to fig. 1 to 5, an embodiment of the present invention provides an ultra-long effective binary slow-release technology for chlorine dioxide, including the following steps:
1) Preparing a saturated acid solution, and adding a powder molecular sieve into the saturated acid solution for soaking, wherein the soaking time is 24 hours, and the weight ratio of the powder molecular sieve to the saturated acid solution is 1-1;
2) Carrying out solid-liquid separation on the soaked molecular sieve, and roasting the molecular sieve after the solid-liquid separation at the roasting temperature of 200-800 ℃ for 2-5 h to obtain a modified molecular sieve;
3) Repeating the steps 1) and 2) for three times, wherein the two steps are used for storing acidic substances in the molecular sieve to the maximum extent by utilizing the adsorbability of the molecular sieve;
4) Coating and drying sodium chlorite powder, wherein the content of sodium chlorite in the sodium chlorite powder is more than or equal to 85 percent, and the granularity range of the sodium chlorite is 50-100 meshes; the coating material is one of sodium alginate and povidone; according to the weight ratio of the sodium chlorite powder to the sodium alginate of 5:1, drying the sodium chlorite powder and povidone according to a weight ratio of 5-10 to obtain coated sodium chlorite, wherein the drying temperature is 80-120 ℃;
5) And (2) mixing the modified molecular sieve, the coated sodium chlorite, the sodium carboxymethylcellulose and the water-absorbing resin according to the weight ratio of 17:4:3:1, mixing and processing to obtain powder A;
6) Adding purified water into the powder A, wherein the weight ratio of the purified water to the powder A is 1.
In a preferred embodiment, the saturated acid solution is one or more of hydrochloric acid, sulfuric acid, nitric acid, oxalic acid and citric acid.
In a preferred embodiment, the powder molecular sieve is 300-600 mesh.
In a preferred embodiment, the roasting temperature is 200-800 ℃, and the roasting time is 2-5 h.
In a preferred embodiment, the content of sodium chlorite in the sodium chlorite powder is more than or equal to 85 percent, and the particle size of the sodium chlorite ranges from 50 meshes to 100 meshes; the coating material is one of sodium alginate and povidone; according to the weight ratio of the sodium chlorite powder to the sodium alginate of 5:1, drying the sodium chlorite powder and povidone according to the weight ratio of 5-10 to obtain coated sodium chlorite, wherein the drying temperature is 80-120 ℃.
In a preferred embodiment, the modified molecular sieve, the coated sodium chlorite, the sodium carboxymethyl cellulose and the water-absorbing resin are mixed according to the weight ratio of 17:4:3:1, mixing for no less than 30 minutes;
in a preferred embodiment, the weight ratio of the purified water to the powder A is 1.
The ultra-long-acting binary slow-release technology for chlorine dioxide controls the reaction period of the acidic substance and sodium chlorite by the saturation of the solution after the slow-release agent is prepared, thereby controlling the generation amount of chlorine dioxide. Due to the saturation of the solution, when the acidic solution is saturated, the acidic substances adsorbed by the molecular sieve cannot be dissolved continuously, so that the residual sodium chlorite cannot react any more, and when the concentration of the acidic substances in the solution is reduced, the acidic substances adsorbed by the molecular sieve start to be dissolved continuously, react with the residual sodium chlorite continuously, and further react continuously to generate chlorine dioxide, so that the generation amount of the chlorine dioxide is increased greatly. Under the condition of lacking moisture, the moisture can be supplemented to dissolve the acidic substances adsorbed by the molecular sieve so as to achieve the aim of continuously releasing chlorine dioxide gas; by the technology, the ultra-long slow release capability of 6-12 months can be realized, and the existing slow release period is improved by 6-12 times.
The invention detects the content of chlorine dioxide:
(1) Detection method
Accurately weigh 2g of sample to an accuracy of 0.0002g. Placing the weighed sample in a 250mL iodine measuring flask in which 2g of potassium iodide is added in advance, and uniformly mixing; adding 20mL of 1; titrating with a sodium thiosulfate standard solution, adding 1mL of starch indicating solution when the end point is reached, continuing to titrate until the blue color disappears, and recording the consumption milliliter number V1 of the sodium thiosulfate standard solution; a blank test was also conducted, and the consumption of ml of the sodium thiosulfate standard solution was recorded as V0. The chlorine dioxide content X in the sample is calculated as follows:
X＝[(△V×C×13.49)÷1000/0.1m]×100
Δ V = V1-V2-is the difference between the volume of sodium thiosulfate for titration and the blank volume, mL;
c-is the actual concentration of the sodium thiosulfate standard solution, mol/L;
m is the sample weight and g is the weight unit;
13.49 is a conversion factor equivalent to the weight of chlorine dioxide consumed for 1ml of a 1mol/L standard solution of sodium thiosulfate.
(2) The chlorine dioxide content of each sample is shown in figure 2.
The finished product stability detection test of the invention:
(1) Detection method
(1) The test method comprises the following steps: taking the packaged finished product, and placing in a constant temperature oven at 37 ℃ for 3 months. The chlorine dioxide content is measured before and after the placement.
(2) And (4) evaluating the results: if the sample is stored at 37 ℃ for 3 months, the reduction rate of the chlorine dioxide content is less than or equal to 15 percent, and the validity period can be set as 2 years.
(2) Stability test results
The content reduction rate of the active ingredient (chlorine dioxide) of the finished product is 7.65 percent (15 percent) after the finished product is stored for 3 months at 37 ℃ according to the stability detection method, the test design requirement is met, and the storage period can be determined to be 2 years.
The finished product of the invention has the following sterilization performance tests:
(1) Preparation of the test
Sealing the cabin: an airtight space with a volume of 1.0m3 (120 cm × 85cm × 100 cm) is provided with an airflow disturbing fan, and an operation port is arranged at a position 30cm away from the bottom layer outside the cabin.
Strains and concentration: the experimental strain is staphylococcus albus; according to the specification of the disinfection technical specification (2008), the concentration of bacteria in the space in the closed cabin is 5 multiplied by 104 to 5 multiplied by 106cfu/m3. Therefore, before the test, the dilution factor of the staphylococcus albus bacterial suspension is determined to meet the regulation on the concentration of the air bacteria in the closed cabin.
(2) Method for contamination with bacteria
Pouring the white staphylococcus bacterium suspension diluted to the specified concentration into an atomizer, and carrying out bacterial contamination for 40min by using a microbial aerosol generator in a closed cabin. After the contamination, the fan continuously disturbs for 5min, and then stands still for 5min;
a liquid impact type microorganism aerosol sampler is applied to carry out bacteria sampling in a closed cabin, wherein the sampling liquid is sterilized 20ml of phosphate buffer solution, 2-3 drops of olive oil (the splashing of the sampling liquid can be prevented) are added, the sampling liquid is poured into a liquid impact bottle for sampling for 10min, the sampling flow is 11L/min and is marked as first sampling, and after 2 hours, the second sampling is carried out by the same method;
1ml of the sampled sample liquid is taken by a pipette on a sterile workbench and is spread on a sterile flat plate. Spreading 2 plates on each sample solution, uniformly sampling, pouring sterilized nutrient agar culture medium onto the plates, cooling, and culturing in 37 deg.C incubator for 48 hr. Counting the colonies on the plate; preparing 4 blank culture mediums for the same batch of samples
Plates, incubated simultaneously with the test samples, served as negative controls.
(3) Sterilization test
(1) 20g of slow-release type immobilized chlorine dioxide particles are filled in a breathable bag and suspended in a closed cabin. The fan is turned on intermittently. Sampling and detecting after 2, 5, 8, 12 and 24 hours respectively.
(2) Pouring 20mL of phosphate buffer solution dropwise added with 2-3 drops of olive oil into a liquid impact bottle, sampling for 10min in two closed cabins by using a liquid impact type microorganism aerosol sampler respectively, wherein the sampling flow rate is 11L/min, spreading 1mL of the sampled sample solution on a sterile workbench by using a liquid transfer gun each time on a sterilized flat plate, then pouring sterilized nutrient agar culture medium added with a neutralizer into the flat plate, spreading 2 flat plates on each sample solution, placing the flat plate in an incubator at 37 ℃ after cooling, and culturing for 48 hours, and calculating the bacterial killing rate.
(4) Test results
As can be seen from FIG. 3, the bacteria killing rate in 12 hours reaches 99.95%, and bacteria and viruses in the air can be killed quickly and effectively.
The finished product of the invention has the degradation performance on formaldehyde
(1) Preparation of the test
Sealing the cabin: volume of 1.0m 3 An air flow disturbing fan is arranged in a closed space (120 cm multiplied by 85cm multiplied by 100 cm), and an operation opening is arranged at a position 30cm away from the bottom layer outside the cabin.
Preparation of formaldehyde gas: a certain amount of formaldehyde solution is measured and placed on an evaporating dish, and the evaporating dish is placed in a closed cabin for fumigation. And after the formaldehyde solution is completely evaporated, continuing turning on the airflow disturbing fan for 5min. The formaldehyde concentration was detected using an L2 hexa-in-one air detector.
(2) Test method
The finished product of the invention is placed in a closed cabin, a fan is in an intermittent opening state, an L2 six-in-one air detector is used for detecting the concentration of formaldehyde at different times, and the removal rate of the finished product to the formaldehyde is calculated.
(3) Results of the experiment
As can be seen from FIG. 4, the finished product of the present invention can effectively degrade formaldehyde, a harmful substance.
As can be seen from figure 5, the detection of the slow release period of the finished product (the release rate of chlorine dioxide is more than 180 mug/h) has the advantages of ultra-long release capability and long slow release period.
In the description of the present specification, the terms "connect", "mount", "fix", and the like are to be understood broadly, for example, "connect" may be a fixed connection, a detachable connection, or an integral connection; may be directly connected or indirectly connected through an intermediate. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In the description of the present application, the description of the terms "one embodiment," "some embodiments," etc. means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (7)
1. A chlorine dioxide saturated slow release technology with super long-term efficiency is characterized by comprising the following steps:
1) Preparing a saturated acid solution, and adding a powder molecular sieve into the saturated acid solution for soaking, wherein the soaking time is 24 hours, and the weight ratio of the powder molecular sieve to the saturated acid solution is 1-1;
2) Carrying out solid-liquid separation on the soaked molecular sieve, and roasting the molecular sieve after the solid-liquid separation at the roasting temperature of 200-800 ℃ for 2-5 h to obtain the modified molecular sieve;
3) Repeating the steps 1) and 2) for three times, wherein the two steps are used for storing acidic substances in the molecular sieve to the maximum extent by utilizing the adsorbability of the molecular sieve;
4) Coating and drying sodium chlorite powder, wherein the content of sodium chlorite in the sodium chlorite powder is more than or equal to 85 percent, and the granularity range of the sodium chlorite is 50-100 meshes; the coating material is one of sodium alginate and povidone; according to the weight ratio of the sodium chlorite powder to the sodium alginate of 5:1, drying the sodium chlorite powder and povidone according to a weight ratio of 5-10 to obtain coated sodium chlorite, wherein the drying temperature is 80-120 ℃;
5) The modified molecular sieve, the coated sodium chlorite, the sodium carboxymethylcellulose and the water-absorbing resin are mixed according to the weight ratio of 17:4:3:1, mixing and processing to obtain powder A;
6) Adding purified water into the powder A, wherein the weight ratio of the purified water to the powder A is 1.
2. The ultra-long-acting chlorine dioxide saturated slow-release technology according to claim 1), characterized in that the saturated acid solution is: including but not limited to one or more of hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, and citric acid.
3. The saturated slow release technology of chlorine dioxide with ultra-long efficiency of claim 2), characterized in that the calcination temperature and time are controlled, and the powder molecular sieve is 300-600 mesh.
4. The saturated slow release technology of chlorine dioxide with ultra-long efficiency according to claim 3), characterized in that the molecular sieve is used to adsorb acidic substances to the maximum extent.
5. The saturated slow-release technology of chlorine dioxide with super-long effectiveness according to claim 4), characterized in that the content of sodium chlorite in the sodium chlorite powder is more than or equal to 85 percent, and the particle size of the sodium chlorite ranges from 50 meshes to 100 meshes; the weight ratio of the sodium chlorite powder to the sodium alginate is 5:1, drying the sodium chlorite powder and povidone according to the weight ratio of 5-10 to obtain coated sodium chlorite, wherein the drying temperature is 80-120 ℃.
6. The saturated slow release technology of chlorine dioxide with super long efficiency according to claim 5), characterized in that the modified molecular sieve, the coated sodium chlorite, the sodium carboxymethylcellulose and the water absorption resin are mixed according to the weight ratio of 17:4:3:1, mixing for no less than 30 minutes.
7. The ultra-long-acting chlorine dioxide saturated slow-release technology according to claim 6), wherein the weight ratio of the purified water to the powder A is 1.
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| CN202210080297.1A CN115363022A (en) | 2022-01-24 | 2022-01-24 | Chlorine dioxide saturation slow-release technology with super-long-acting performance |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118062809A (en) * | 2024-04-22 | 2024-05-24 | 山东高密高源化工有限公司 | Preparation method of sodium chlorite |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118062809A (en) * | 2024-04-22 | 2024-05-24 | 山东高密高源化工有限公司 | Preparation method of sodium chlorite |
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Application publication date: 20221122 |