阅读说明：本技术 一种过硫酸氢钾复合盐粉消毒剂的制备方法及其制备的过硫酸氢钾复合盐粉消毒剂和应用 (Preparation method of potassium hydrogen persulfate composite salt powder disinfectant, potassium hydrogen persulfate composite salt powder disinfectant prepared by using same and application of potas) 是由 张许科 师梦超 于 2019-10-21 设计创作，主要内容包括：本发明提供了一种制备过硫酸氢钾复合物粉消毒剂的方法,本发明制备方法通过对组方中部分辅料进行干法制粒,显著提高了粉末流动性和稳定性,且改善了粉末的扬尘性；同时对矫味剂、着色剂、氯化钠和过硫酸氢钾复合物粉分别预混合,实现了过硫酸氢钾复合物粉颜色和气味的均匀性,以及避免了氯化钠被过硫酸氢钾复合物粉氧化的问题。本发明制备方法工艺简单,对设备要求低,有利于规模化生产。(The invention provides a method for preparing a potassium hydrogen persulfate composite powder disinfectant, wherein the preparation method of the potassium hydrogen persulfate composite powder disinfectant remarkably improves the flowability and stability of the powder and improves the dust emission of the powder by performing dry granulation on part of auxiliary materials in a formula; meanwhile, the flavoring agent, the coloring agent, the sodium chloride and the potassium hydrogen persulfate composite powder are respectively premixed, so that the uniformity of the color and the odor of the potassium hydrogen persulfate composite powder is realized, and the problem that the sodium chloride is oxidized by the potassium hydrogen persulfate composite powder is solved. The preparation method has simple process and low requirement on equipment, and is beneficial to large-scale production.)

1. A method of preparing a oxone complex powder disinfectant, wherein the method comprises: sieving raw materials of a potassium hydrogen persulfate composite powder disinfectant, wherein the raw materials of the potassium hydrogen persulfate composite powder disinfectant comprise: 40-60 w/w% of potassium hydrogen persulfate composite salt, 3-10 w/w% of sulfamic acid, 0.5-5.0 w/w% of sodium chloride, 5-20 w/w% of surfactant, 5-20 w/w% of acidifying agent, 10-20 w/w% of water softener, 0.5-10 w/w% of cosolvent, 0.01-0.5 w/w% of flavoring agent and 0.03-1.5 w/w% of coloring agent;

respectively premixing the flavoring agent and the coloring agent with 10 w/w% of prescription amount of potassium hydrogen persulfate composite salt;

step (3) mixing sodium chloride with 10 w/w% of prescription amount of potassium hydrogen persulfate composite salt by a double division method;

step (4), carrying out dry granulation on the surfactant and the water softener;

step (5) putting the residual amount of the potassium hydrogen persulfate composite salt, all the untreated auxiliary materials and the products prepared in the steps (3) and (4) into a mixer for mixing; and

and (6) putting the product prepared in the step (2) and the product prepared in the step (5) into a mixer for mixing to obtain the potassium hydrogen persulfate composite powder disinfectant.

2. The method of claim 1, wherein the acidulant is one or more of malic acid, tartaric acid, citric acid, fumaric acid; the water softener is one or more of sodium hexametaphosphate, sodium tripolyphosphate, EDTA-2Na and sodium gluconate; the cosolvent is one or more of PEG6000, poloxamer, PVPK30 and hydroxypropyl beta-cyclodextrin; the surfactant is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and sodium dodecyl sulfate; the flavoring agent is lemon essential oil or limonene; the colorant is amaranth pigment.

3. The method of claim 2 wherein the oxone complex powder disinfectant feed comprises: 50 w/w% of potassium hydrogen persulfate composite salt, 13 w/w% of sodium dodecyl benzene sulfonate, 1.5 w/w% of sodium chloride, 5 w/w% of sulfamic acid, 18 w/w% of sodium hexametaphosphate, 10 w/w% of malic acid, 0.08 w/w% of amaranth, 0.4 w/w% of lemon essential oil, EDTA-2Na0.02 w/w% and PEG60002.0 w/w%.

4. The oxone complex powder disinfectant as defined in claim 2 wherein the oxone complex disinfectant raw material comprises: the oxone complex powder comprises: 50 w/w% of potassium hydrogen persulfate composite salt, 2 w/w% of sodium chloride, 10 w/w% of malic acid, 5 w/w% of sulfamic acid, 15 w/w% of sodium dodecyl benzene sulfonate, 0.03 w/w% of EDTA-2Na, 15 w/w% of sodium hexametaphosphate, 2.4 w/w% of hydroxypropyl beta cyclodextrin, 0.5 w/w% of lemon essential oil and 0.07 w/w% of amaranth.

5. The method of claim 2 wherein the oxone complex powder disinfectant feed comprises: the oxone complex powder comprises: 50 w/w% of potassium hydrogen persulfate composite salt, 2 w/w% of sodium chloride, 5 w/w% of sulfamic acid, 13 w/w% of sodium dodecyl benzene sulfonate, 0.75 w/w% of EDTA-2Na, 10 w/w% of citric acid, 15 w/w% of sodium hexametaphosphate, PEG 60004 w/w%, 0.1 w/w% of amaranth and 0.15 w/w% of limonene.

6. The method of claim 2 wherein the oxone complex powder disinfectant feed comprises: 50 w/w% of potassium hydrogen persulfate composite salt, 2 w/w% of sodium chloride, 5 w/w% of sulfamic acid, 13 w/w% of sodium dodecyl benzene sulfonate, 0.55 w/w% of sodium gluconate, 0.2 w/w% of EDTA-2Na, 10 w/w% of malic acid, 14 w/w% of sodium hexametaphosphate, 5 w/w% of PVP, 0.1 w/w% of amaranth and 0.15 w/w% of limonene.

7. The method of claim 2 wherein the oxone complex powder disinfectant feed comprises: 53 w/w% of potassium hydrogen persulfate composite salt, 1.5 w/w% of sodium chloride, 3 w/w% of sulfamic acid, 13 w/w% of sodium dodecyl benzene sulfonate, 5.75 w/w% of sodium tripolyphosphate, 8.5 w/w% of malic acid, 10 w/w% of sodium hexametaphosphate, 5 w/w% of poloxamer, 0.1 w/w% of amaranth and 0.15 w/w% of limonene.

8. The method of claim 2 wherein the oxone complex powder disinfectant feed comprises: 55 w/w% of potassium hydrogen persulfate composite salt, 1.5 w/w% of sodium chloride, 5 w/w% of sulfamic acid, 13 w/w% of sodium dodecyl benzene sulfonate, 10 w/w% of sodium tripolyphosphate, 5 w/w% of fumaric acid, 4.75 w/w% of sodium hexametaphosphate, 5 w/w% of hydroxypropyl beta-cyclodextrin, 0.1 w/w% of amaranth and 0.15 w/w% of limonene.

9. The oxone complex powder disinfectant prepared by the method according to claims 1-8.

10. Use of the oxone complex powder disinfectant of claim 9 in the disinfection of livestock and poultry environment.

Technical Field

The invention belongs to the field of veterinary medicines, and particularly relates to a preparation method of a potassium hydrogen persulfate composite powder disinfectant, the prepared potassium hydrogen persulfate composite powder disinfectant and application.

Background

Frequent outbreaks of infectious diseases of livestock and poultry not only cause huge loss to animal husbandry, but also threaten the healthy life of people, so that the prevention and treatment of the infectious diseases of the livestock and poultry have very important public health significance. In the epidemic disease prevention and control link, the disinfectant is one of important means. Most of the currently used chemical disinfectants are single disinfectant, such as phenol, formaldehyde, glutaraldehyde, ethanol, bleaching powder, and the like. The single disinfectant has respective disadvantages, such as poor stability, inconvenient use, toxicity, large irritation or serious corrosivity, narrow antibacterial spectrum and the like. And the single-component disinfectant for animals has limited disinfection effect and is easily influenced by organic matters, temperature, water quality and environmental pH value, wherein aldehydes also have the possibility of carcinogenicity.

The potassium hydrogen persulfate complex powder (compound peroxisome sulfate powder) is a mixture composed of peroxide, halide, surfactant, organic acid and inorganic buffer system with stable equilibrium, and its main ingredients are potassium hydrogen persulfate complex salt (KMPS) and sodium chloride. The veterinary compound disinfectant has high-efficiency killing effect on viruses, bacteria, fungi, mycoplasma, spores and other microorganisms, is a broad-spectrum, low-toxicity and non-hazardous chemical product, does not endanger human health, can be used at low temperature and has organic matter interference resistance.

CN108184828A uses inert powder and hydrophobic agent to perform moisture-proof and anti-caking of potassium hydrogen persulfate composite powder, although this method can solve the problem of moisture absorption and caking property of powder, the inert powder and hydrophobic agent generally have poor solubility in water, which can cause the composite powder to be turbid or semitransparent in water, and affect the apparent property of solution. CN101828550A discloses a composite potassium hydrogen persulfate powder disinfection tablet which has broad-spectrum sterilization and virus killing effects. The formula process is simple and easy to produce. However, as the raw materials and the auxiliary materials are directly mixed and tableted, the sodium chloride is easily oxidized by the potassium hydrogen persulfate composite salt to generate chlorine gas to volatilize in the storage process, so that the effective components are reduced. CN101836659A adopts a new process, and hydroxypropyl cellulose, hydroxypropyl methylcellulose, polyvinylpyrrolidone, ethyl cellulose and the like are selected as film coatings, so that the irritation and hygroscopicity of the product are solved, but the process is complex and the requirement on equipment is high. CN108184828A improves the fluidity, stability and appearance uniformity of the potassium hydrogen persulfate composite powder by co-coloring part of the auxiliary materials in the formula and adjusting the adding and stirring sequence of the main materials and the auxiliary materials. Some other methods adopt special processes to increase the stability of the potassium hydrogen persulfate composite powder, such as sodium chloride coating technology (CN106942271A), sustained-release framework (CN105360162A) and the like. In CN106942271A, sodium chloride is coated with a sodium chloride wrap compounded by alkyl glycoside and sodium alginate, so that sodium chloride is prevented from being oxidized by potassium hydrogen persulfate composite salt, the stability of the product is remarkably improved, and the storage life is prolonged. Although the methods can improve the stability of the potassium hydrogen persulfate composite powder to a certain extent, the methods have the disadvantages of complicated technology, high requirements on equipment and cost and respective defects. In addition, most patent formulas are based on a DuPont patent US4822512, the stability and the anti-caking property of the potassium hydrogen persulfate composite powder are solved by adding an anti-caking agent, a hydrophobic agent or part of auxiliary materials, and the dust emission problem of the powder is not solved all the time. In WO9103936A1, in order to solve the stability and applicability of potassium hydrogen persulfate composite powder, effervescent agents and adhesives are added to perform tabletting on the composite powder to prepare effervescent tablets, although the stability and dust raising problems of the disinfectant are improved, the effervescent agents are sodium carbonate, and double decomposition reaction is easy to occur between the effervescent agents and main materials and partial auxiliary materials in the storage process, so that the stability of the preparation is influenced.

Disclosure of Invention

The invention integrates the technical defects, and provides a safe, effective, stable, anti-caking and simple-process preparation method of the potassium hydrogen persulfate composite powder.

The invention provides a method for preparing a potassium hydrogen persulfate composite powder disinfectant, which comprises the following steps: sieving raw materials of a potassium hydrogen persulfate composite powder disinfectant, wherein the raw materials of the potassium hydrogen persulfate composite powder disinfectant comprise: 40-60 w/w% of potassium hydrogen persulfate composite salt, 3-10 w/w% of sulfamic acid, 0.5-5.0 w/w% of sodium chloride, 5-20 w/w% of surfactant, 5-20 w/w% of acidifying agent, 10-20 w/w% of water softener, 0.5-10 w/w% of cosolvent, 0.01-0.5 w/w% of flavoring agent and 0.03-1.5 w/w% of coloring agent; respectively premixing the flavoring agent and the coloring agent with 10 w/w% of prescription amount of potassium hydrogen persulfate composite salt; step (3) mixing sodium chloride with 10 w/w% of prescription amount of potassium hydrogen persulfate composite salt by a double division method; step (4), carrying out dry granulation on the surfactant and the water softener; and step (5) putting the residual amount of the potassium hydrogen persulfate composite salt, all auxiliary materials and the products prepared in the steps (3) and (4) into a mixer for mixing; and (3) putting the product prepared in the step (2) and the product prepared in the step (5) into a mixer for mixing to obtain the potassium hydrogen persulfate composite powder disinfectant.

Different from the prior art of adding the anti-caking agent in the potassium hydrogen persulfate composite powder, the preparation method provided by the invention has the advantages that partial auxiliary materials in the formula are subjected to dry granulation, so that the powder flowability and stability are obviously improved, and the dust emission of the powder is improved. The invention realizes the uniformity of color and smell of the potassium hydrogen persulfate composite powder by respectively premixing the flavoring agent, the coloring agent, the sodium chloride and the potassium hydrogen persulfate composite powder, avoids the problem that the sodium chloride is oxidized by the potassium hydrogen persulfate composite powder, does not generate gas, and ensures the stability of the content of the effective chlorine and the sodium chloride in the disinfectant under the conditions of long-term placement, high temperature and high humidity.

The preparation method has simple process and low requirement on equipment, and is beneficial to large-scale production. The invention not only optimizes the prescription of the disinfectant, but also adds the preparation process steps, thereby solving the problem that the uniformity of the color and the odor of the potassium hydrogen persulfate compound powder is not consistent. The potassium hydrogen persulfate composite powder obtained by the invention is safe, effective, stable, anti-caking and uniform in coloring, and is easy for large-scale production.

The content of the potassium hydrogen persulfate composite salt in the raw material of the potassium hydrogen persulfate composite powder disinfectant can be selected from 40 w/w%, 41 w/w%, 42 w/w%, 43 w/w%, 44 w/w%, 45 w/w%, 46 w/w%, 47 w/w%, 48 w/w%, 49 w/w%, 50 w/w%, 51 w/w%, 52 w/w%, 53 w/w%, 54 w/w%, 55 w/w%, 56 w/w%, 57 w/w%, 58 w/w%, 59 w/w% and 60 w/w%.

The content of sulfamic acid can be selected from 3 w/w%, 4 w/w%, 5 w/w%, 6 w/w%, 7 w/w%, 8 w/w%, 9 w/w%, 10 w/w%.

The sodium chloride content may be selected from 0.5 w/w%, 0.6 w/w%, 0.7 w/w%, 0.8 w/w%, 0.9 w/w%, 1.0 w/w%, 2.0 w/w%, 2.5 w/w%, 3.0 w/w%, 3.5 w/w%, 4.0 w/w%, 4.5 w/w%, 5.0 w/w%.

The surfactant content may be selected from 5 w/w%, 6 w/w%, 7 w/w%, 8 w/w%, 9 w/w%, 10 w/w%, 11 w/w%, 12 w/w%, 13 w/w%, 14 w/w%, 15 w/w%, 16 w/w%, 17 w/w%, 18 w/w%, 19 w/w%, 20 w/w%.

The acidulant content may be selected from 5 w/w%, 6 w/w%, 7 w/w%, 8 w/w%, 9 w/w%, 10 w/w%, 11 w/w%, 12 w/w%, 13 w/w%, 14 w/w%, 15 w/w%, 16 w/w%, 17 w/w%, 18 w/w%, 19 w/w%, 20 w/w%.

The water softener content may be selected from 10 w/w%, 11 w/w%, 12 w/w%, 13 w/w%, 14 w/w%, 15 w/w%, 16 w/w%, 17 w/w%, 18 w/w%, 19 w/w%, 20 w/w%.

The co-solvent content may be selected from 0.5 w/w%, 0.6 w/w%, 0.7 w/w%, 0.8 w/w%, 0.9 w/w%, 1.0 w/w%, 2.0 w/w%, 3.0 w/w%, 4.0 w/w%, 5.0 w/w%, 6.0 w/w%, 7.0 w/w%, 8.0 w/w%, 9.0 w/w%, 10 w/w%.

The content of the flavoring agent can be selected from 0.01 w/w%, 0.02 w/w%, 0.03 w/w%, 0.04 w/w%, 0.05 w/w%, 0.06 w/w%, 0.07 w/w%, 0.08 w/w%, 0.09 w/w%, 0.1 w/w%, 0.2 w/w%, 0.3 w/w%, 0.4 w/w%, 0.5 w/w%.

The colorant content may be selected from 0.03 w/w%, 0.04 w/w%, 0.05 w/w%, 0.06 w/w%, 0.07 w/w%, 0.08 w/w%, 0.09 w/w%, 0.1 w/w%, 0.2 w/w%, 0.3 w/w%, 0.4 w/w%, 0.5 w/w%, 0.6 w/w%, 0.7 w/w%, 0.8 w/w%, 0.9 w/w%, 1.0 w/w%, 1.1 w/w%, 1.2 w/w%, 1.3 w/w%, 1.4 w/w%, 1.5 w/w%.

In one embodiment of the present invention, in the preparation method of the potassium hydrogen persulfate compound powder disinfectant, the acidulant is one or more of malic acid, tartaric acid, citric acid and fumaric acid; the water softener is one or more of sodium hexametaphosphate, sodium tripolyphosphate, EDTA-2Na and sodium gluconate; the cosolvent is one or more of PEG6000, poloxamer, PVPK30 and hydroxypropyl beta-cyclodextrin; the surfactant is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and sodium dodecyl sulfate; the flavoring agent is lemon essential oil or limonene; the colorant is amaranth pigment.

In a preferred embodiment of the present invention, in the method for preparing a potassium persulfate complex powder disinfectant according to the present invention, the raw material of the potassium persulfate complex powder disinfectant comprises: 50 w/w% of potassium hydrogen persulfate composite salt, 13 w/w% of sodium dodecyl benzene sulfonate, 1.5 w/w% of sodium chloride, 5 w/w% of sulfamic acid, 18 w/w% of sodium hexametaphosphate, 10 w/w% of malic acid, 0.08 w/w% of amaranth, 0.4 w/w% of lemon essential oil, EDTA-2Na0.02 w/w% and PEG60002.0 w/w%.

In a preferred embodiment of the present invention, in the method for preparing a potassium persulfate complex powder disinfectant according to the present invention, the raw material of the potassium persulfate complex powder disinfectant comprises: the oxone complex powder comprises: 50 w/w% of potassium hydrogen persulfate composite salt, 2 w/w% of sodium chloride, 10 w/w% of malic acid, 5 w/w% of sulfamic acid, 15 w/w% of sodium dodecyl benzene sulfonate, 0.03 w/w% of EDTA-2Na, 15 w/w% of sodium hexametaphosphate, 2.4 w/w% of hydroxypropyl beta cyclodextrin, 0.5 w/w% of lemon essential oil and 0.07 w/w% of amaranth.

In a preferred embodiment of the present invention, in the method for preparing a potassium persulfate complex powder disinfectant according to the present invention, the raw material of the potassium persulfate complex powder disinfectant comprises: the oxone complex powder comprises: 50 w/w% of potassium hydrogen persulfate composite salt, 2 w/w% of sodium chloride, 5 w/w% of sulfamic acid, 13 w/w% of sodium dodecyl benzene sulfonate, 0.75 w/w% of EDTA-2Na, 10 w/w% of citric acid, 15 w/w% of sodium hexametaphosphate, PEG 60004 w/w%, 0.1 w/w% of amaranth and 0.15 w/w% of limonene.

In a preferred embodiment of the present invention, in the method for preparing a potassium persulfate complex powder disinfectant according to the present invention, the raw material of the potassium persulfate complex powder disinfectant comprises: 50 w/w% of potassium hydrogen persulfate composite salt, 2 w/w% of sodium chloride, 5 w/w% of sulfamic acid, 13 w/w% of sodium dodecyl benzene sulfonate, 0.55 w/w% of sodium gluconate, 0.2 w/w% of EDTA-2Na, 10 w/w% of malic acid, 14 w/w% of sodium hexametaphosphate, 5 w/w% of PVP, 0.1 w/w% of amaranth and 0.15 w/w% of limonene.

In a preferred embodiment of the present invention, in the method for preparing a potassium persulfate complex powder disinfectant according to the present invention, the raw material of the potassium persulfate complex powder disinfectant comprises: 53 w/w% of potassium hydrogen persulfate composite salt, 1.5 w/w% of sodium chloride, 3 w/w% of sulfamic acid, 13 w/w% of sodium dodecyl benzene sulfonate, 5.75 w/w% of sodium tripolyphosphate, 8.5 w/w% of malic acid, 10 w/w% of sodium hexametaphosphate, 5 w/w% of poloxamer, 0.1 w/w% of amaranth and 0.15 w/w% of limonene.

In a preferred embodiment of the present invention, in the method for preparing a potassium persulfate complex powder disinfectant according to the present invention, the raw material of the potassium persulfate complex powder disinfectant comprises: 55 w/w% of potassium hydrogen persulfate composite salt, 1.5 w/w% of sodium chloride, 5 w/w% of sulfamic acid, 13 w/w% of sodium dodecyl benzene sulfonate, 10 w/w% of sodium tripolyphosphate, 5 w/w% of fumaric acid, 4.75 w/w% of sodium hexametaphosphate, 5 w/w% of hydroxypropyl beta-cyclodextrin, 0.1 w/w% of amaranth and 0.15 w/w% of limonene.

The invention also relates to the potassium hydrogen persulfate composite powder disinfectant prepared by the method. The potassium hydrogen persulfate composite powder prepared by the method has excellent stability and caking resistance, does not cake when stored under the conditions of high temperature and high humidity, and the effective components are kept stable.

The powder disinfectant prepared by the method is detected according to the detection requirements under the item of the potassium hydrogen persulfate composite powder in the quality standard of imported veterinary drugs, the effective rate content of the powder disinfectant is 10.5 w/w-13 w/w%, the sodium chloride content is 1.2 w/w-1.5 w/w%, the pH value of 1% aqueous solution is 2.35-2.65, and the sodium dodecyl benzene sulfonate thin layer is qualified.

The potassium hydrogen persulfate composite powder disinfectant overcomes the defect that a single disinfectant is inconvenient to use, is safe, effective, stable, anti-caking, free of dust raising and gas generation, uniform in coloring, simple in production process and low in cost, and meets the requirements of veterinary drug quality assembly 2006 plus 2011, and the quantitative production in a workshop is easy to realize.

The invention also provides application of the potassium hydrogen persulfate composite powder disinfectant in livestock and poultry environment disinfection.

The aqueous solution prepared from the potassium hydrogen persulfate composite powder is stable in content of active ingredients after being placed for about one week, and the solution has good disinfection and sterilization effects on the environment of livestock and poultry farms.

Detailed Description

The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.

The chemical reagents used in the examples of the present invention are all analytical reagents and purchased from the national pharmaceutical group. The experimental methods are conventional methods unless specified otherwise; the biomaterial is commercially available unless otherwise specified.

Preparation example 1 preparation of Potassium Hydrogen persulfate composite powder according to the invention

This example of oxonium persulfate complex powder (1kg) was prepared from the following raw materials: 500g of potassium hydrogen persulfate composite salt, 20g of sodium chloride, 50g of sulfamic acid, 130g of sodium dodecyl benzene sulfonate, 7.5g of EDTA-2Na, 100g of citric acid, 150g of sodium hexametaphosphate, PEG 600040 g, 1g of amaranth and 1.5g of limonene.

The preparation method comprises the following steps:

sieving raw materials: sieving all solid materials except amaranth with 24 mesh sieve for use.

Premixing: premixing amaranth, lemon essential oil and sodium chloride with 10 w/w% of potassium hydrogen persulfate composite salt, and mixing for 5min, wherein the sodium chloride is mixed by a double division method.

And (3) dry granulation: sodium dodecyl benzene sulfonate and sodium hexametaphosphate are granulated by a dry method.

Mixing raw materials and auxiliary materials: firstly, sodium hexametaphosphate, sulfamic acid, sodium dodecyl benzene sulfonate, EDTA-2Na, citric acid, PEG6000 and premixed sodium chloride are put into a mixer to be mixed for 20 min.

And adding the premixed amaranth and lemon essential oil into a mixer for mixing for 30 min.

Subpackaging and packaging: transferring part of the composite powder in the mixer to a packaging machine for debugging, and packaging after the packaging amount is qualified; and transferring to a packaging room for packaging and warehousing after subpackaging.

Preparation of example 2

This example of oxonium persulfate complex powder (1kg) was prepared from the following raw materials: 500g of potassium hydrogen persulfate composite salt, 20g of sodium chloride, 50g of sulfamic acid, 130g of sodium dodecyl benzene sulfonate, 5.5g of sodium gluconate, 2g of EDTA-2Na, 100g of malic acid, 140g of sodium hexametaphosphate, 50g of PVP, 1g of amaranth and 1.5g of limonene.

The preparation method refers to the preparation method of example 1 to prepare the anti-caking and dust-free potassium hydrogen persulfate composite powder.

Preparation of example 3

This example of oxonium persulfate complex powder (1kg) was prepared from the following raw materials: 530g of potassium hydrogen persulfate composite salt, 15g of sodium chloride, 30g of sulfamic acid, 130g of sodium dodecyl benzene sulfonate, 57.5g of sodium tripolyphosphate, 85g of malic acid, 100g of sodium hexametaphosphate, 50g of poloxamer, 1g of amaranth and 1.5g of limonene.

The preparation method refers to the preparation method of example 1 to prepare the anti-caking and dust-free potassium hydrogen persulfate composite powder.

Preparation of example 4

This example of oxonium persulfate complex powder (1kg) was prepared from the following raw materials: 550g of potassium hydrogen persulfate composite salt, 15g of sodium chloride, 50g of sulfamic acid, 130g of sodium dodecyl benzene sulfonate, 100g of sodium tripolyphosphate, 50g of fumaric acid, 47.5g of sodium hexametaphosphate, 50g of hydroxypropyl beta-cyclodextrin, 1g of amaranth and 1.5g of limonene.

The preparation method refers to the preparation method of example 1 to prepare the anti-caking and dust-free potassium hydrogen persulfate composite powder.

Preparation of comparative example 1

This comparative example oxonium persulfate composite powder (1kg) was prepared from the following raw materials: 500g of potassium hydrogen persulfate composite salt, 20g of sodium chloride, 50g of sulfamic acid, 130g of sodium dodecyl benzene sulfonate, 7.5g of EDTA-2Na, 100g of citric acid, 100g of sodium hexametaphosphate, 50g of sodium tripolyphosphate, 40g of poloxamer, 1g of amaranth and 1.5g of limonene.

The preparation method comprises the following steps:

after the raw and auxiliary materials are sieved by a 24-mesh sieve, firstly, mixing sodium hexametaphosphate and sodium dodecyl benzene sulfonate, then performing dry granulation, sequentially putting the potassium hydrogen persulfate composite salt, citric acid, sulfamic acid, EDTA-2Na, poloxamer, sodium chloride and limonene, the sodium dodecyl benzene sulfonate, the sodium hexametaphosphate and the prepared granules into a mixer for mixing for 40min, and then performing split charging and packaging to obtain the potassium hydrogen persulfate composite powder prepared in the comparative example 1.

Preparation of comparative example 2

This comparative example oxonium persulfate composite powder (1kg) was prepared from the following raw materials: 578g of potassium hydrogen persulfate composite salt, 20g of sodium chloride, 50g of sulfamic acid, 100g of sodium dodecyl benzene sulfonate, 80g of malic acid, 150g of sodium hexametaphosphate, 20g of anhydrous sodium citrate, 1.0g of amaranth and 1.0g of limonene.

The preparation method comprises the following steps: after sieving the raw and auxiliary materials by a 24-mesh sieve, sequentially putting the potassium hydrogen persulfate composite salt, the malic acid, the sulfamic acid, the sodium hexametaphosphate, the sodium chloride, the sodium dodecyl benzene sulfonate, the anhydrous sodium citrate, the limonene and the amaranth into a mixer for mixing for 40min, and then subpackaging and packaging to obtain the potassium hydrogen persulfate composite powder prepared in the comparative example 2.

Example 5 quality control of Potassium Hydrogen persulfate composite powders prepared in preparation examples 1 to 4 of the present invention and preparation comparative examples 1 and 2

The quality of the oxonium persulfate composite powder prepared in the preparation examples 1 to 4 and the preparation comparative examples 1 to 2 was measured in three parallel samples according to the test item of oxonium persulfate composite powder in the veterinary drug quality assembly 2006-2011 edition, and the test results of each sample are shown in table 1:

TABLE 1 quality testing of the oxonium persulfate composite powders of the present invention and controls

The test results show that the potassium hydrogen persulfate composite powder prepared by the method has uniform color and uniform powder mixing, and the quality detection results of the times are consistent. The product prepared without dyeing premixing and orderly mixing of raw materials and auxiliary materials has nonuniform color and granularity, the powder is not easy to mix uniformly, and the difference of each quality detection result is large.

Therefore, the steps of coloring premixing, sodium chloride doubling, dry granulation and raw and auxiliary material feeding sequence have important influence on the appearance and the character of the product, the caking condition and the powder uniformity. Compared with the traditional powder direct mixing process, the method disclosed by the embodiment of the invention has the advantages that the prepared product has better properties, more uniform content and more reliable quality.

Experimental example 2 Experimental detection of influencing factors

The results of the influential factor tests conducted on the oxonium persulfate composite powders prepared in the preparation examples 1 to 4 and the preparation comparative examples 1 to 2, respectively, are shown in the following table, in which table 2 is the experimental result of the influence of high temperature (40 ℃) on the stability, and table 3 is the experimental result of the influence of high humidity (25 ℃, 90 ± 5% RH) on the stability:

TABLE 2 high temperature influencing factor test

TABLE 3 high humidity Effect factor test

As can be seen from tables 2 and 3, the oxone complex powder prepared by the method of the present invention has excellent stability and anti-caking property, no caking occurs even when the powder is stored under high temperature and high humidity conditions, and the effective components are kept stable;

according to the detection results of the preparation examples and the preparation comparative examples, the application of the dry granulation technology of the auxiliary materials which are easy to absorb moisture can effectively improve the stability and the tolerance to the environmental humidity of the potassium hydrogen persulfate composite powder, and the better moisture-proof effect can be achieved by matching the application of the water softeners such as sodium tripolyphosphate and the like.

Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.