CN111903674B - Potassium hydrogen persulfate composite powder with uniform and stable quality and preparation process thereof - Google Patents
Potassium hydrogen persulfate composite powder with uniform and stable quality and preparation process thereof Download PDFInfo
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- CN111903674B CN111903674B CN202010778200.5A CN202010778200A CN111903674B CN 111903674 B CN111903674 B CN 111903674B CN 202010778200 A CN202010778200 A CN 202010778200A CN 111903674 B CN111903674 B CN 111903674B
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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
- A01N25/12—Powders or granules
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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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- 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
- A01N59/02—Sulfur; Selenium; Tellurium; Compounds thereof
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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
- A01N59/08—Alkali metal chlorides; Alkaline earth metal chlorides
Abstract
The invention relates to the field of pharmaceutical chemicals, and particularly relates to uniform and stable-quality potassium hydrogen persulfate composite powder and a preparation process thereof. The potassium hydrogen persulfate composite powder comprises the following components: potassium hydrogen persulfate complex, sulfamic acid, sodium hexametaphosphate, sodium dodecyl benzene sulfonate, sodium chloride, anti-caking agent and trisodium citrate; also comprises essence and pigment. The potassium hydrogen persulfate composite powder is superior to the potassium hydrogen persulfate composite powder on the market, the process is simple, and the cost is hardly increased; the appearance color and luster is uniform and consistent, the content is uniform, the user can conveniently use the disinfection solution to monitor the effective disinfection concentration in real time in clinic, the product is not layered in the transportation process, and the product quality is more stable. The process can adopt closed integrated equipment for production in actual production, greatly reduces pollution to people and environment, and is a direction for safe and environment-friendly production in future.
Description
Technical Field
The invention relates to the field of pharmaceutical chemicals, and particularly relates to uniform and stable-quality potassium hydrogen persulfate composite powder and a preparation process thereof.
Background
The potassium hydrogen persulfate composite powder is an environment-friendly disinfectant which is broad-spectrum, efficient, reliable, durable and safe and consists of potassium hydrogen persulfate, sodium chloride and the like. Has high-efficiency killing effect on pathogenic microorganisms such as bacteria, viruses, fungi, mycoplasma and the like. The national epidemic control departments such as the United states, the United kingdom and the like approve the use of the potassium hydrogen persulfate composite powder for the prevention and control of major epidemic situations, and the potassium hydrogen persulfate composite powder is also the first and the only veterinary disinfectant approved and registered by the environmental protection department of the United states for preventing the foot-and-mouth disease. The 'technical guide for recovery of production of infected African swine fever farms' newly released by the animal husbandry and veterinary administration of rural agricultural departments in China approves one of disinfectants effective to African swine fever viruses.
Compared with the common powder, the potassium hydrogen persulfate composite powder has the following two characteristics: (1) the pH value has influence on the stability of the product, and the pH value of the product is required to be between 2.35 and 2.65 in the quality standard; (2) the effective disinfection concentration is indicated through color change, and when the color of the disinfectant solution with a certain concentration is changed from color to colorless, the concentration of the disinfectant is indicated to be incapable of meeting the disinfection requirement, so that a user can conveniently and directly master the disinfection effect.
At present, most of the varieties in the market are prepared by a simple powder mixing process. As the potassium hydrogen persulfate composite powder has more components and different properties, and the particle size, the fluidity and the particle size difference are larger, the products on the market mainly have three problems: (1) the uniformity of the color of the amaranth is poor due to the fine granularity and poor fluidity of the amaranth; (2) because of the granularity graduation difference of materials and the brittleness difference of the materials, particularly, the sodium dodecyl benzene sulfonate is a surfactant, is not easy to crush and is easy to agglomerate, and the appearance uniformity and the internal quality of a product are influenced; (3) the above two problems further affect the internal quality of the product, make the pH value of the product unstable, make the uniformity of chloride and content poor, and directly affect the stability and disinfection effect of the product.
But relevant documents on how to improve the stability, the appearance uniformity and the influence of pH on the stability of the potassium hydrogen persulfate composite powder disinfectant are not available at present. The problems are mentioned in only some documents and patents (application number CN201711470217.9) on the potassium hydrogen persulfate composite powder for preventing agglomeration and a preparation method and application thereof, the emphasis is mainly on prescription adjustment, but the problems cannot be fundamentally solved according to the characteristics of amaranth, sodium dodecyl benzene sulfonate and other materials in the prescription. The problem can be solved fundamentally only by changing the process according to the properties of the materials.
Disclosure of Invention
Aiming at the defects and the defects of the appearance color uniformity of the existing potassium hydrogen persulfate composite powder, the invention changes the fluidity and the granularity of two materials by adding the anti-caking agent which is easy to disperse into the sodium dodecyl benzene sulfonate and the pigment and crushing and mixing the materials, so that the materials meet the process requirements; or adding an easily dispersible anticaking agent into sodium dodecyl benzene sulfonate, pulverizing, mixing to change its fluidity and granularity, and making pigment into uniform solution to change color nonuniformity. The two methods aim to provide the potassium hydrogen persulfate composite powder with uniform and stable quality, the appearance color is uniform, the content is uniform, the quality is stable, and the potassium hydrogen persulfate composite powder is not layered after shaking, so that the quality of the potassium hydrogen persulfate composite powder is improved, the effective concentration in clinical use is ensured, and the capability of killing viruses and bacteria is further ensured.
The invention is realized by the following technical scheme:
a oxone complex powder comprising the components of: potassium hydrogen persulfate complex, sulfamic acid, sodium hexametaphosphate, sodium dodecylbenzenesulfonate, sodium chloride, anticaking agent, and trisodium citrate.
Further, the potassium hydrogen persulfate compound is 2KHSO5·KHSO4·K2SO4。
Further, the anticaking agent is selected from one or more of silicon dioxide, calcium phosphate, calcium silicate, calcium stearate, cellulose, kaolin, magnesium carbonate, magnesium hydroxide, magnesium silicate, magnesium stearate, sodium ferrocyanide, sodium aluminosilicate, sodium calcium aluminosilicate, sucrose ester and calcium aluminosilicate.
Furthermore, the components of the potassium hydrogen persulfate composite powder also comprise essence and pigment. Furthermore, the essence is selected from one or a mixture of more than two of lemon essence, corn essence, grapefruit essence, orange essence, cherry essence, apple essence, strawberry essence, milk essence and coconut essence; the pigment is selected from amaranth, roselle, safflower yellow, caramel, carmine, erythrosine, new red, rose bengal, lemon yellow, sunset yellow, brilliant blue and indigo blue, or a mixture of two or more of them.
Further, the formula of the potassium hydrogen persulfate composite powder is as follows: 50-70% (g/g) of potassium hydrogen persulfate compound; 2-6% (g/g) of sulfamic acid; 12-18% (g/g) of sodium hexametaphosphate; 3-8% (g/g) of sodium dodecyl benzene sulfonate; 3-5% (g/g) of sodium chloride; 1-3% (g/g) of essence; 0.1-0.5% (g/g) of pigment; 0.2-1.0% (g/g) of an anti-caking agent; 6-9% (g/g) of trisodium citrate.
Furthermore, the formula of the potassium hydrogen persulfate composite powder is as follows: 60-65% (g/g) of potassium hydrogen persulfate compound; 4% (g/g) sulfamic acid; 13-16% (g/g) of sodium hexametaphosphate; 5 percent (g/g) of sodium dodecyl benzene sulfonate; 3.9% (g/g) of sodium chloride; 2% of essence (g/g); pigment 0.3% (g/g); 0.3-0.8% (g/g) of an anti-caking agent; trisodium citrate 6.5-8.0% (g/g).
Still further, the formula of the potassium hydrogen persulfate composite powder is as follows: 62% (g/g) of potassium hydrogen persulfate complex; sulfamic acid 4% (g/g); 14.5% (g/g) of sodium hexametaphosphate; 5 percent (g/g) of sodium dodecyl benzene sulfonate; 3.9% (g/g) of sodium chloride; 2% of essence (g/g); pigment 0.3% (g/g); 0.8 percent of anticaking agent (g/g); trisodium citrate 7.5% (g/g).
The invention also provides a preparation method of the potassium hydrogen persulfate composite powder, which comprises the following steps:
(1) respectively pulverizing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving;
(2) respectively sieving the essence and the potassium hydrogen persulfate compound for later use;
(3) respectively weighing the sodium chloride and the sulfamic acid in the step (1) and the essence in the step (2) according to the prescription, and uniformly mixing for later use;
(4) weighing sodium hexametaphosphate in the step (1) and trisodium citrate according to the prescription, and uniformly mixing for later use;
(5) weighing sodium dodecyl benzene sulfonate, an anti-caking agent and a pigment according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing uniformly;
(7) and finally, adding the potassium hydrogen persulfate compound with the prescription amount into the step (6) and uniformly mixing to obtain the potassium hydrogen persulfate compound powder with uniform and stable quality.
Further, the preparation method of the potassium hydrogen persulfate composite powder comprises the following steps:
(1) respectively pulverizing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving;
(2) respectively sieving the essence and the potassium hydrogen persulfate compound for later use;
(3) respectively weighing the sodium chloride and the sulfamic acid in the step (1) and the essence in the step (2) according to the prescription, and mixing for 10min for later use;
(4) weighing sodium hexametaphosphate in the step (1) according to a formula and mixing with trisodium citrate for 10min for later use;
(5) weighing sodium dodecyl benzene sulfonate, an anticaking agent and a pigment according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing for 15 min;
(7) and finally, adding the prescription amount of the potassium hydrogen persulfate compound into the mixture obtained in the step (6) and mixing for 15min to obtain the potassium hydrogen persulfate compound powder with uniform and stable quality.
Further, the sieving in the preparation method is a 65-mesh sieving.
The invention also provides another preparation method of the potassium hydrogen persulfate composite powder, which comprises the following steps:
(1) respectively pulverizing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving;
(2) respectively sieving the essence and the potassium hydrogen persulfate compound for later use;
(3) respectively weighing sodium chloride and sulfamic acid in the step (1) and essence in the step (2) according to the prescription, and uniformly mixing for later use;
(4) weighing sodium hexametaphosphate in the step (1) according to the prescription, and uniformly mixing the sodium hexametaphosphate with trisodium citrate for later use;
(5) weighing sodium dodecyl benzene sulfonate and an anti-caking agent according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing uniformly;
(7) adding the hydrogen potassium persulfate compound with the amount of the prescription into the step (6) and uniformly mixing;
(8) dissolving pigment in appropriate amount of solvent to obtain pigment solution;
(9) uniformly spraying (8) into (7);
(10) and (7) drying to obtain the uniform and stable quality potassium hydrogen persulfate composite powder.
Further, the preparation method of the potassium hydrogen persulfate composite powder comprises the following steps:
(1) respectively crushing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving with a 65-mesh sieve for later use;
(2) respectively sieving the essence and the potassium hydrogen persulfate compound by a 65-mesh sieve for later use;
(3) respectively weighing sodium chloride and sulfamic acid in the step (1) and essence in the step (2) according to the prescription, and mixing for 10min for later use;
(4) weighing sodium hexametaphosphate in the step (1) according to a formula and mixing with trisodium citrate for 10min for later use;
(5) weighing sodium dodecyl benzene sulfonate and an anti-caking agent according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing for 15 min;
(7) adding the prescription amount of the potassium hydrogen persulfate compound into the mixture (6) and mixing for 15 min;
(8) dissolving pigment in appropriate amount of solvent to obtain pigment solution;
(9) uniformly spraying (8) into (7);
(10) and (4) drying the (7) at 50 ℃ for 4 hours to obtain the uniform and stable quality potassium hydrogen persulfate composite powder.
Further, in the step (8), the solvent is one or more selected from purified water, ethanol, methanol, chloroform and ethyl acetate.
The invention has the beneficial effects that:
the potassium hydrogen persulfate composite powder is superior to the potassium hydrogen persulfate composite powder on the market, the process is simple, and the cost is hardly increased; the appearance color and luster is uniform and consistent, the content is uniform, the user can conveniently use the disinfection solution to monitor the effective disinfection concentration in real time in clinic, the product is not layered in the transportation process, and the product quality is more stable. The process can adopt closed integrated equipment for production in actual production, greatly reduces pollution to people and environment, and is a direction for safe and environment-friendly production in future.
Drawings
FIG. 1 is a graph comparing the appearance of samples prepared in examples 1 and 2 with 2 batches prepared by a conventional powder process. From left to right are the sample prepared in example 1, the sample prepared in example 2, control 1, and control 2, respectively.
Detailed Description
The technical solutions of the present invention are further illustrated by the following specific embodiments, but it is easily understood by those skilled in the art that the specific material ratios, process conditions and results thereof described in the examples are only for illustrating the present invention, and should not also limit the present invention described in detail in the claims.
Example 1
The preparation process of potassium hydrogen persulfate composite powder with homogeneous and stable quality includes the following steps:
6.2kg of potassium hydrogen persulfate compound counted by 10kg of potassium hydrogen persulfate compound powder; 0.4kg of sulfamic acid; 1.45kg of sodium hexametaphosphate; 0.5kg of sodium dodecyl benzene sulfonate; 0.39kg of sodium chloride; 0.2kg of lemon essence; 0.03kg of amaranth pigment; 0.08kg of silicon dioxide and 0.75kg of trisodium citrate.
(1) Respectively pulverizing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving;
(2) sieving lemon essence and potassium hydrogen persulfate compound respectively for later use;
(3) respectively weighing sodium chloride and sulfamic acid in the step (1) and lemon essence in the step (2) according to the prescription, and mixing for 10min for later use;
(4) weighing sodium hexametaphosphate in the step (1) according to a formula and mixing with trisodium citrate for 10min for later use;
(5) weighing sodium dodecyl benzene sulfonate, silicon dioxide and amaranth pigment according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing for 15 min;
(7) finally, adding the prescription amount of the potassium hydrogen persulfate compound into the mixture obtained in the step (6) and mixing for 15min to obtain light pink potassium hydrogen persulfate compound powder;
(8) detecting an intermediate;
(9) subpackaging, sealing, and labeling to obtain the final product.
Example 2
The preparation method of the potassium hydrogen persulfate composite powder with uniform and stable quality comprises the following steps:
6.2kg of potassium hydrogen persulfate compound counted by 10kg of potassium hydrogen persulfate compound powder; 0.4kg of sulfamic acid; 1.45kg of sodium hexametaphosphate; 0.5kg of sodium dodecyl benzene sulfonate; 0.39kg of sodium chloride; 0.2kg of lemon essence; 0.03kg of amaranth pigment; 0.08kg of silicon dioxide; 0.75kg of trisodium citrate; 1kg of purified water.
(1) Respectively crushing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving with a 65-mesh sieve for later use;
(2) respectively sieving the lemon essence and the potassium hydrogen persulfate compound by a 65-mesh sieve for later use;
(3) respectively weighing sodium chloride and sulfamic acid in the step (1) and lemon essence in the step (2) according to the prescription, and mixing for 10min for later use;
(4) weighing sodium hexametaphosphate in the step (1) according to the prescription, and mixing with trisodium citrate for 10min for later use;
(5) weighing sodium dodecyl benzene sulfonate and silicon dioxide according to the proportion of the prescription, mixing and crushing for later use;
(6) mixing the above (3), (4) and (5) for 15 min;
(7) adding the prescription amount of the potassium hydrogen persulfate compound into the mixture (6) and mixing for 15 min;
(8) dissolving amaranth in a proper amount of solvent (50% ethanol), and preparing into pigment solution;
(9) uniformly spraying (8) into (7);
(10) drying the powder obtained in the step (7) at 50 ℃ for 4 hours to obtain the potassium hydrogen persulfate composite powder with uniform color and appearance;
(11) detecting an intermediate;
(12) subpackaging, sealing, and labeling to obtain the final product.
Example 3
The preparation method of the potassium hydrogen persulfate composite powder with uniform and stable quality comprises the following steps:
5.0kg of potassium hydrogen persulfate compound counted by 10kg of potassium hydrogen persulfate compound powder; 0.6kg of sulfamic acid; 1.8kg of sodium hexametaphosphate; 0.8kg of sodium dodecyl benzene sulfonate; 0.5kg of sodium chloride; 0.25kg of lemon essence; 0.05kg of amaranth pigment; 0.1kg of silicon dioxide; 0.9kg of trisodium citrate.
The preparation method is the same as example 1.
Example 4
The preparation method of the potassium hydrogen persulfate composite powder with uniform and stable quality comprises the following steps:
7.0kg of potassium hydrogen persulfate compound counted by 10kg of potassium hydrogen persulfate compound powder; 0.3kg of sulfamic acid; 1.3kg of sodium hexametaphosphate; 0.3kg of sodium dodecyl benzene sulfonate; 0.3kg of sodium chloride; 0.1kg of lemon essence; 0.01kg of amaranth pigment; 0.09kg of silicon dioxide; 0.6kg of trisodium citrate; and a proper amount of purified water.
The preparation method is the same as example 2, and the solvent is 50% ethanol replaced by purified water.
Example 5
The preparation method of the potassium hydrogen persulfate composite powder with uniform and stable quality comprises the following steps:
6.0kg of potassium hydrogen persulfate compound counted by 10kg of potassium hydrogen persulfate compound powder; 0.4kg of sulfamic acid; 1.6kg of sodium hexametaphosphate; 0.5kg of sodium dodecyl benzene sulfonate; 0.39kg of sodium chloride; 0.2kg of lemon essence; 0.03kg of amaranth pigment; 0.08kg of silicon dioxide; 0.8kg of trisodium citrate.
The preparation method is the same as example 1.
Example 6
The preparation method of the potassium hydrogen persulfate composite powder with uniform and stable quality comprises the following steps:
6.5kg of potassium hydrogen persulfate compound counted by 10kg of potassium hydrogen persulfate compound powder; 0.4kg of sulfamic acid; 1.3kg of sodium hexametaphosphate; 0.5kg of sodium dodecyl benzene sulfonate; 0.39kg of sodium chloride; 0.2kg of lemon essence; 0.03kg of amaranth pigment; 0.03kg of silicon dioxide; 0.65kg of trisodium citrate; proper amount of 50% ethanol.
The preparation method is the same as example 2.
Comparative example 1
The potassium hydrogen persulfate composite powder with uniform and stable quality and the preparation process thereof comprise the following steps:
6.2kg of potassium hydrogen persulfate compound counted by 10kg of potassium hydrogen persulfate compound powder; 0.4kg of sulfamic acid; 1.45kg of sodium hexametaphosphate; 0.5kg of sodium dodecyl benzene sulfonate; 0.39kg of sodium chloride; 0.2kg of lemon essence; 0.03kg of amaranth pigment; 0.08kg of silicon dioxide and 0.75kg of trisodium citrate.
(1) Respectively pulverizing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving;
(2) sieving sodium dodecyl benzene sulfonate, lemon essence, silicon dioxide, amaranth pigment and potassium hydrogen persulfate compound respectively for later use;
(3) respectively weighing sodium chloride and sulfamic acid which are crushed and sieved in the step (1) and sodium dodecyl benzene sulfonate, lemon essence, silicon dioxide and amaranth pigment which are sieved in the step (2) according to the prescription, and mixing for 10min for later use;
(4) weighing the powder and the sieved sodium hexametaphosphate in the step (1) according to the prescription, and mixing the powder and the trisodium citrate for 10min for later use;
(5) adding the above (3) and (4) and the potassium hydrogen persulfate compound sieved according to the prescription amount, and mixing for 15min to obtain pink potassium hydrogen persulfate compound powder;
(6) detecting an intermediate;
(7) subpackaging, sealing, and labeling to obtain the final product.
Comparative example 2
The potassium hydrogen persulfate composite powder with uniform and stable quality and the preparation process thereof comprise the following steps:
6.2kg of potassium hydrogen persulfate compound counted by 10kg of potassium hydrogen persulfate compound powder; 0.4kg of sulfamic acid; 1.45kg of sodium hexametaphosphate; 0.5kg of sodium dodecyl benzene sulfonate; 0.39kg of sodium chloride; 0.2kg of lemon essence; 0.03kg of amaranth pigment; 0.83kg of trisodium citrate.
(1) Sieving sodium hexametaphosphate, trisodium citrate, sulfamic acid, sodium chloride and potassium hydrogen persulfate compound respectively for later use;
(2) weighing sodium dodecyl benzene sulfonate, lemon essence and amaranth pigment according to the prescription respectively for later use;
(3) respectively weighing the sieved sodium chloride and sulfamic acid in the step (1) according to the prescription, adding the sodium dodecyl benzene sulfonate, the lemon essence and the amaranth pigment in the step (2), and mixing for 10min for later use;
(4) adding the sodium hexametaphosphate weighed in the step (1) and trisodium citrate into the step (3) according to the prescription, and mixing for 10min for later use;
(5) adding the hydrogen potassium persulfate compound with the prescription amount into the step (4), and mixing for 15min to obtain light pink hydrogen potassium persulfate compound powder;
(6) detecting an intermediate;
(7) subpackaging, sealing and labeling to obtain the finished product.
Test example 1
The samples prepared in examples 1 and 2 and the two controls prepared in comparative example 1 and comparative example 2 (control 1 and control 2, respectively) were examined for uniformity of appearance, uniformity of pH, uniformity of sodium chloride and uniformity of content, and after shaking, the samples were examined in their entirety according to the registered standards, wherein 6 samples of pH, sodium chloride and content were examined and the relative standard deviation was calculated. The results are shown in Table 1, and the uniformity of appearance is shown in FIG. 1.
TABLE 1 results of the related index tests of the samples prepared in examples 1-2 and comparative examples 1-2
As can be seen from the results in table 1 and fig. 1, the indexes associated with 4 samples all meet the registration standard. However, from the RSD in table 1, it can be seen that the oxone composite powders prepared according to examples 1 and 2 of the present invention have good color uniformity, pH, sodium chloride content and uniform distribution of available chlorine, which are significantly superior to similar products prepared by the conventional process.
Accelerated stability tests were performed on 3 batches of each sample prepared in examples 1 and 2, and the results are shown in tables 2 and 3 below. The result shows that the stability test result of 6 months shows that the potassium hydrogen persulfate composite powder prepared according to the changed process conditions of the invention has uniform appearance and color and stable internal quality.
TABLE 2 test results of accelerated testing of 3 batches of oxone composite powder prepared in example 1
Table 3 accelerated test results for 3 batches of oxone composite powder prepared in example 2
Claims (10)
1. The potassium hydrogen persulfate composite powder is characterized in that the formula of the potassium hydrogen persulfate composite powder is as follows: 50-70% (g/g) of potassium hydrogen persulfate compound; 2-6% (g/g) of sulfamic acid; 12-18% (g/g) of sodium hexametaphosphate; 3-8% (g/g) of sodium dodecyl benzene sulfonate; 3-5% (g/g) of sodium chloride; 1-3% (g/g) of essence; 0.1-0.5% (g/g) of pigment; 0.2-1.0% (g/g) of an anti-caking agent; 6-9% (g/g) of trisodium citrate;
the preparation method of the potassium hydrogen persulfate composite powder comprises the following steps:
(1) respectively pulverizing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving;
(2) respectively sieving the essence and the potassium hydrogen persulfate compound for later use;
(3) respectively weighing the sodium chloride and the sulfamic acid in the step (1) and the essence in the step (2) according to the prescription, and uniformly mixing for later use;
(4) weighing sodium hexametaphosphate in the step (1) and trisodium citrate according to the prescription, and uniformly mixing for later use;
(5) weighing sodium dodecyl benzene sulfonate, an anti-caking agent and a pigment according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing uniformly;
(7) finally, adding the prescription amount of the potassium hydrogen persulfate compound into the step (6) and uniformly mixing to obtain the potassium hydrogen persulfate compound powder with uniform and stable quality;
the pigment is amaranth.
2. The oxonium persulfate composite powder according to claim 1, wherein the formulation of the oxonium persulfate composite powder is: 60-65% (g/g) of potassium hydrogen persulfate compound; sulfamic acid 4% (g/g); 13-16% (g/g) of sodium hexametaphosphate; 5 percent (g/g) of sodium dodecyl benzene sulfonate; 3.9% (g/g) of sodium chloride; 2% of essence (g/g); pigment 0.3% (g/g); 0.3-0.8% (g/g) of an anti-caking agent; trisodium citrate 6.5-8.0% (g/g).
3. The oxone complex powder of claim 1, wherein the formulation of the oxone complex powder is: 62% (g/g) of potassium hydrogen persulfate complex; sulfamic acid 4% (g/g); sodium hexametaphosphate 14.5% (g/g); 5 percent (g/g) of sodium dodecyl benzene sulfonate; 3.9% (g/g) of sodium chloride; 2% of essence (g/g); pigment 0.3% (g/g); 0.8 percent of anticaking agent (g/g); trisodium citrate 7.5% (g/g).
4. The oxone complex powder according to claim 1, wherein the preparation method comprises the steps of:
(1) respectively pulverizing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving;
(2) respectively sieving the essence and the potassium hydrogen persulfate compound for later use;
(3) respectively weighing the sodium chloride and the sulfamic acid in the step (1) and the essence in the step (2) according to the prescription, and mixing for 10min for later use;
(4) weighing sodium hexametaphosphate in the step (1) according to a formula and mixing with trisodium citrate for 10min for later use;
(5) weighing sodium dodecyl benzene sulfonate, an anti-caking agent and a pigment according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing for 15 min;
(7) and finally, adding the prescription amount of the potassium hydrogen persulfate compound into the mixture obtained in the step (6) and mixing for 15min to obtain the potassium hydrogen persulfate compound powder with uniform and stable quality.
5. The oxone complex powder according to any one of claims 1 to 4, wherein the preparation process comprises the steps of: the sieving in the preparation method is to sieve with 65 meshes.
6. The potassium hydrogen persulfate composite powder is characterized in that the formula of the potassium hydrogen persulfate composite powder is as follows: 50-70% (g/g) of potassium hydrogen persulfate compound; 2-6% (g/g) of sulfamic acid; 12-18% (g/g) of sodium hexametaphosphate; 3-8% (g/g) of sodium dodecyl benzene sulfonate; 3-5% (g/g) of sodium chloride; 1-3% (g/g) of essence; 0.1-0.5% (g/g) of pigment; 0.2-1.0% (g/g) of an anti-caking agent; 6-9% (g/g) of trisodium citrate;
the preparation method of the potassium hydrogen persulfate composite powder comprises the following steps:
(1) respectively pulverizing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving;
(2) respectively sieving the essence and the potassium hydrogen persulfate compound for later use;
(3) respectively weighing sodium chloride and sulfamic acid in the step (1) and essence in the step (2) according to the prescription, and uniformly mixing for later use;
(4) weighing sodium hexametaphosphate in the step (1) and trisodium citrate according to the prescription, and uniformly mixing for later use;
(5) weighing sodium dodecyl benzene sulfonate and an anti-caking agent according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing uniformly;
(7) adding the hydrogen potassium persulfate compound with the amount of the prescription into the step (6) and uniformly mixing;
(8) dissolving pigment in appropriate amount of solvent to obtain pigment solution;
(9) uniformly spraying (8) into (7);
(10) drying the (7) to obtain the potassium hydrogen persulfate composite powder with uniform and stable quality;
the pigment is amaranth.
7. The oxonium persulfate composite powder according to claim 6, wherein the formulation of the oxonium persulfate composite powder is: 60-65% (g/g) of potassium hydrogen persulfate compound; sulfamic acid 4% (g/g); 13-16% (g/g) of sodium hexametaphosphate; 5 percent (g/g) of sodium dodecyl benzene sulfonate; 3.9% (g/g) of sodium chloride; 2% of essence (g/g); pigment 0.3% (g/g); 0.3-0.8% (g/g) of an anti-caking agent; trisodium citrate 6.5-8.0% (g/g).
8. The oxonium persulfate composite powder according to claim 6, wherein the formulation of the oxonium persulfate composite powder is: 62% (g/g) of potassium hydrogen persulfate complex; sulfamic acid 4% (g/g); sodium hexametaphosphate 14.5% (g/g); 5 percent (g/g) of sodium dodecyl benzene sulfonate; 3.9% (g/g) of sodium chloride; 2% of essence (g/g); pigment 0.3% (g/g); 0.8 percent of anticaking agent (g/g); trisodium citrate 7.5% (g/g).
9. The oxone complex powder according to claim 6, wherein the preparation method comprises the steps of:
(1) respectively crushing sodium hexametaphosphate, trisodium citrate, sulfamic acid and sodium chloride, and sieving with a 65-mesh sieve for later use;
(2) respectively sieving essence and potassium hydrogen persulfate compound with 65 mesh sieve;
(3) respectively weighing sodium chloride and sulfamic acid in the step (1) and essence in the step (2) according to the prescription, and mixing for 10min for later use;
(4) weighing sodium hexametaphosphate in the step (1) according to a formula and mixing with trisodium citrate for 10min for later use;
(5) weighing sodium dodecyl benzene sulfonate and an anti-caking agent according to the proportion of the prescription, mixing and crushing for later use;
(6) adding the above (3), (4) and (5) and mixing for 15 min;
(7) adding the prescription amount of the potassium hydrogen persulfate compound into the mixture (6) and mixing for 15 min;
(8) dissolving pigment in appropriate amount of solvent to obtain pigment solution;
(9) uniformly spraying (8) into (7);
(10) and (4) drying the (7) at 50 ℃ for 4 hours to obtain the potassium hydrogen persulfate composite powder with uniform and stable quality.
10. The oxone complex powder according to any one of claims 6 to 9, wherein the solvent in step (8) is one or more selected from purified water, ethanol, methanol, chloroform, ethyl acetate.
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| CN113287627B (en) * | 2021-05-25 | 2021-12-17 | 中山市迈微环保科技有限公司 | Cleaning disinfectant containing potassium hydrogen persulfate compound, and use method and application thereof |
| CN113383790A (en) * | 2021-07-23 | 2021-09-14 | 湖南加农正和生物技术有限公司 | Environment-friendly potassium hydrogen persulfate compound disinfectant and production process thereof |
| CN113383791A (en) * | 2021-07-23 | 2021-09-14 | 湖南微草生物饲料科技有限公司 | Reinforced potassium hydrogen persulfate compound disinfectant and preparation process thereof |
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