A kind of halquinol suspension and preparation method thereof

Abstract

The invention relates to a halquinol suspension and a preparation method thereof. The halquinol suspension comprises the following raw materials calculated by mass percentage: 1% to 20% of halquinol, 0.05% to 2% of a suspending agent, 1.5% to 5% of a solubilizing agent, 1% to 5% of an antifreeze agent, 2% to 10% of an auxiliary agent, and the balance is water. The halquinol suspension of the invention does not stratify, settle, or harden after standing for 1 month, and has good fluidity; after standing at -10 to 0°C for 48 hours, no stratification or solidification occurs, and the viscosity changes within a range of 20%, thereby improving the applicable weather conditions of the halquinol suspension.

Description

Technical Field

[0001] The invention belongs to the technical field of feed additives, and particularly relates to a halquinol suspension and a preparation method thereof. Background Art

[0002] Halquinol is a mixture of chlorinated hydroxyquinolines, mainly composed of 5,7-dichloro-8-hydroxyquinoline and 5-chloro-8-hydroxyquinoline. Halquinol can regulate the balance of intestinal microorganisms in livestock and poultry, effectively remove pathogenic Escherichia coli, Salmonella, etc. in the intestine, and control the spread of diseases; it can slow down the peristalsis of the intestines of livestock and poultry, increase the absorption of water and nutrients, thereby improving feed conversion rate and promoting animal growth. In the current livestock market, with the increase in attention to animal and food safety, the demand for natural, residue-free additives such as Halquinol continues to grow. At present, Halquinol is a widely used feed additive in Southeast Asia and South America to promote animal growth and protect the balance of intestinal microecology.

[0003] Based on the physical properties of Halquinol, it is insoluble in water and easy to settle. There is no public stable and uniform dosage form of Halquinol. With the advancement of digital information technology, intelligent breeding has gradually become a new development direction for animal husbandry. In the future, the development trend of Halquinol as a feed additive will focus on combining with digital intelligent breeding. Therefore, we are looking for a quantitative, controllable, and convenient Halquinol dosage form for animals. This Halquinol dosage form can be combined with an intelligent feeding system or an intelligent spraying system to achieve digitally controlled and measurable intelligent dosage control. Summary of the invention

[0004] The first object of the present invention is to provide a halquinol suspension to solve the technical problem that the existing halquinol is difficult to combine with an intelligent breeding system or an intelligent spraying system.

[0005] The second object of the present invention is to provide a method for preparing a halquinol suspension.

[0006] In order to achieve the above purpose, the technical solution adopted by the present invention is:

[0007] The invention discloses a halquinol suspension, which comprises the following raw materials calculated by mass percentage: 1% to 20% of halquinol, 0.05% to 2% of a suspending agent, 1.5% to 5% of a solubilizing agent, 1% to 5% of an antifreeze agent, 2% to 10% of an auxiliary agent, and the balance is water.

[0008] Furthermore, the halquinol comprises the following raw materials: 57% to 74% by mass of 5,7-dichloro-8-hydroxyquinoline, 23% to 40% by mass of 5-chloro-8-hydroxyquinoline and 0% to 4% by mass of 7-chloro-8-hydroxyquinoline.

[0009] Furthermore, the dynamic viscosity of the halquinol suspension is 85 to 160 mPa·s.

[0010] Furthermore, the particle size of the halquinol suspension is 100 to 200 μm.

[0011] Furthermore, the suspending agent is a polymer suspending agent; the solubilizing agent is an ionic surfactant; the antifreeze agent is a sugar antifreeze agent; and the auxiliary agent is a ternary weak acid and its derivatives.

[0012] Furthermore, the suspending agent is a cellulose suspending agent; the solubilizing agent is an anionic surfactant; the antifreeze agent is a small molecule sugar antifreeze agent; and the auxiliary agent is one or more of citric acid and sodium citrate.

[0013] Furthermore, the suspending agent is one or more of methyl cellulose, sodium carboxymethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and hydroxyethyl cellulose; the solubilizing agent is one or more of sodium dodecyl sulfate and sodium dodecylbenzene sulfonate; and the antifreeze agent is one or more of sucrose, lactose, maltose, and trehalose.

[0014] A preparation method of a halquinol suspension comprises the following steps: mixing the halquinol, a suspending agent, a solubilizing agent, an antifreeze agent and an auxiliary agent in a formula amount to obtain a solid powder, crushing the solid powder to obtain a dry suspension, and sieving the dry suspension and stirring and mixing it with a formula amount of water to obtain the suspension.

[0015] Furthermore, the mesh size of the sieve through which the dry suspension is screened is 100 to 200 meshes.

[0016] Furthermore, the stirring speed is 200-2000 r / min; the stirring temperature is 10-30°C.

[0017] Beneficial effects of the present invention:

[0018] The halquinol suspension of the present invention does not stratify, settle or harden after being left standing for one month, and has good fluidity; after being left standing at -10 to 0°C for 48 hours, no stratification or solidification occurs, and the viscosity variation range is within 20%, thereby improving the applicable weather conditions of the halquinol suspension; the particle size of the halquinol suspension prepared by the present invention is between 100 and 500 μm, and the halquinol suspension can be sprayed through a fan-shaped nozzle or a centrifugal nozzle spraying device, and the spraying effect is uniform, and it is convenient to be combined with an intelligent feeding system or an intelligent spraying system, and the purpose of numerical control quantitative can be achieved.

[0019] Cellulose suspending agents and anionic surfactant solubilizing agents can improve the dispersibility and uniformity of halquinol in water; by adding small molecule sugar antifreeze agents, on the one hand, the freezing point of halquinol suspension can be lowered, which is convenient for the preservation of halquinol suspension in winter and improves the stability of halquinol suspension; on the other hand, small molecule sugar antifreeze agents can be used as sweeteners to adjust the taste of halquinol suspension and improve the acceptance of livestock and poultry; by adding citric acid and sodium citrate additives, the gastrointestinal environment can be regulated by adjusting the pH value of halquinol suspension. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is the gas phase detection diagram of the Halquinol suspension in Example 3;

[0021] Figure 2 This is a state diagram of the Halquinol suspension in Example 1-3 after standing for 0 h;

[0022] Figure 3 This is a state diagram of the Halquinol suspension in Example 1-3 after being left to stand for 3 days;

[0023] Figure 4 This is a state diagram of the Halquinol suspension in Example 1-3 after being left to stand for 15 days;

[0024] Figure 5 This is a state diagram of the Halquinol suspension in Example 1-3 after being left to stand for 1 m;

[0025] Figure 6 This is a state diagram of the Halquinol suspension in Example 3 at -10°C for 48 hours;

[0026] Figure 7 This is a test diagram of the spraying uniformity of the Halquinol suspension in Example 3. DETAILED DESCRIPTION

[0027] The present invention will be further described below in conjunction with the embodiments of the present invention and the accompanying drawings.

[0028] Example 1

[0029] The preparation method of the halquinol suspension of Example 1 comprises the following steps: adding 1g of halquinol, 0.05g of methylcellulose, 2g of citric acid, 2g of sodium lauryl sulfate, and 1.05g of sucrose to a suspension instrument and mixing for 20min to obtain a solid powder, crushing the obtained solid powder through a crusher to obtain a dry suspension, passing the dry suspension through a 150-mesh sieve of the R40 / 3 series, adding 93.9g of water, setting the speed to 200r / min, and stirring at 20°C for 30min to obtain a 1% halquinol suspension with a sedimentation ratio of 0.99.

[0030] Halquinol includes 65% by mass of 5,7-dichloro-8-hydroxyquinoline, 29% by mass of 5-chloro-8-hydroxyquinoline and 2.3% by mass of 7-chloro-8-hydroxyquinoline.

[0031] Example 2

[0032] The preparation method of the halquinol suspension of Example 2 comprises the following steps: adding 3g halquinol, 0.3g hydroxyethyl cellulose, 4g sodium citrate, 2.7g sodium dodecylbenzene sulfonate, and 1g maltose to a suspension instrument and mixing for 20min to obtain a solid powder, crushing the obtained solid powder through a crusher to obtain a dry suspension, passing the dry suspension through a 100-mesh sieve of the R40 / 3 series, adding 89g water, setting the speed to 300r / min, and stirring at 22°C for 40min to obtain a 3% halquinol suspension with a sedimentation ratio of 0.99.

[0033] Halquinol includes 71% by mass of 5,7-dichloro-8-hydroxyquinoline, 24% by mass of 5-chloro-8-hydroxyquinoline and 1.9% by mass of 7-chloro-8-hydroxyquinoline.

[0034] Example 3

[0035] The preparation method of the halquinol suspension of Example 3 comprises the following steps: 5g halquinol, 0.5g sodium carboxymethyl cellulose, 6g sodium citrate, 1.5g sodium dodecyl sulfate, and 2.5g lactose are added to a suspension instrument and mixed for 30min to obtain a solid powder, the obtained solid powder is crushed by a crusher to obtain a dry suspension, the dry suspension is passed through a 200-mesh sieve of the R40 / 3 series, 84.5g of water is added, the speed is set to 700r / min, and stirred at 25°C for 30min to obtain a 5% halquinol suspension with a sedimentation ratio of 0.99. The gas phase content detection spectrum of the halquinol suspension of Example 3 is as shown Figure 1 shown.

[0036] Halquinol includes 73% by mass of 5,7-dichloro-8-hydroxyquinoline, 25% by mass of 5-chloro-8-hydroxyquinoline and 0.7% by mass of 7-chloro-8-hydroxyquinoline.

[0037] Example 4

[0038] The preparation method of the halquinol suspension of Example 4 comprises the following steps: adding 7g of halquinol, 1g of hydroxyethyl cellulose, 7g of citric acid, 3g of sodium lauryl sulfate, and 4g of trehalose to a suspension mixer and mixing for 30min to obtain a solid powder, crushing the obtained solid powder through a crusher to obtain a dry suspension, passing the dry suspension through a 200-mesh sieve of the R40 / 3 series, adding 78g of water, setting the speed to 1500r / min, and stirring at 15°C for 10min to obtain a 7% halquinol suspension with a sedimentation ratio of 1.00.

[0039] Halquinol includes 57% by mass of 5,7-dichloro-8-hydroxyquinoline, 40% by mass of 5-chloro-8-hydroxyquinoline and 0.3% by mass of 7-chloro-8-hydroxyquinoline.

[0040] Example 5

[0041] The preparation method of the halquinol suspension of Example 5 comprises the following steps: adding 10g halquinol, 1g hydroxyethyl cellulose, 6g sodium citrate, 3g sodium lauryl sulfate, and 1g sucrose into a suspension mixer and mixing for 20min to obtain a solid powder, crushing the obtained solid powder through a crusher to obtain a dry suspension, passing the dry suspension through a 200-mesh sieve, adding 79g water, setting the speed to 2000r / min, stirring at 10°C for 10min, and obtaining a 10% halquinol suspension with a sedimentation ratio of 0.99.

[0042] Halquinol includes 74% by mass of 5,7-dichloro-8-hydroxyquinoline and 23% by mass of 5-chloro-8-hydroxyquinoline.

[0043] Example 6

[0044] The preparation method of the halquinol suspension of Example 6 comprises the following steps: 15 g of halquinol, 1.5 g of hydroxypropyl cellulose, 8 g of sodium citrate, 4.5 g of sodium lauryl sulfate, and 5 g of sucrose are added to a suspension mixer and mixed for 20 min to obtain a solid powder, the obtained solid powder is crushed by a crusher to obtain a dry suspension, the dry suspension is sieved through a 200 mesh sieve, 66 g of water is added, the speed is set to 1100 r / min, and stirred at 25 ° C for 50 min to obtain a 15% halquinol suspension with a sedimentation ratio of 0.97.

[0045] Halquinol includes 60% by mass of 5,7-dichloro-8-hydroxyquinoline, 35% by mass of 5-chloro-8-hydroxyquinoline and 4% by mass of 7-chloro-8-hydroxyquinoline.

[0046] Example 7

[0047] The preparation method of the halquinol suspension of Example 7 comprises the following steps: adding 20g halquinol, 2g hydroxypropyl methylcellulose, 10g citric acid, 5g sodium dodecylbenzene sulfonate, and 2g trehalose to a suspension mixer and mixing for 20min to obtain a solid powder, crushing the obtained solid powder through a crusher to obtain a dry suspension, passing the dry suspension through a 200-mesh sieve, adding 61g water, setting the speed to 500r / min, and stirring at 30°C for 60min to obtain a 20% halquinol suspension with a sedimentation ratio of 0.96.

[0048] Halquinol includes 65% by mass of 5,7-dichloro-8-hydroxyquinoline, 29% by mass of 5-chloro-8-hydroxyquinoline and 2.3% by mass of 7-chloro-8-hydroxyquinoline.

[0049] Comparative Examples 1-7

[0050] Comparative Examples 1-7 were respectively prepared with 10g of Halquinol suspension of different concentrations, stirred evenly, and then allowed to stand for 12 hours for observation. The raw materials of Halquinol suspension of Comparative Examples 1-7 are shown in Table 1. Halquinol of Comparative Examples 1-7 includes 5,7-dichloro-8-hydroxyquinoline with a mass fraction of 65%, 5-chloro-8-hydroxyquinoline with a mass fraction of 29%, and 7-chloro-8-hydroxyquinoline with a mass fraction of 2.3%.

[0051] Table 1 Raw materials of the Halquinol suspension of Comparative Examples 1-7

[0052]

[0053] As can be seen from Table 1, when only sodium dodecylbenzene sulfonate, sodium dodecyl sulfate or sodium citrate was added, the prepared halquinol suspension was partially dissolved after standing for 12 hours, while the halquinol suspension prepared by adding citric acid, lactose and sodium carboxymethyl cellulose as additives was stratified after standing for 12 hours. Figure 2-Figure 6 It can be seen that the Halquinol suspension prepared by the present invention did not show stratification when left standing at room temperature for 1 month or at -10°C for 48 hours, indicating that the suspending agent, solubilizing agent, antifreeze agent and auxiliary agent of the present invention have a compounding effect, which can improve the stability of the Halquinol suspension.

[0054] Test Example 1

[0055] Stability test

[0056] 2 mL of the halquinol suspension of Example 1-7 was placed at 25°C for 1 day (1d), 3 days (3d), 7 days (7d), 15 days (15d), and 1 month (1m). The halquinol content in the sample was detected by gas chromatography external standard method. The results are shown in Table 2.

[0057] Table 2 The content of halquinol in the halquinol suspension of Examples 1-7 after standing for a certain period of time

[0058]

[0059] It can be seen from Table 2 that the content of the halquinol suspensions of Examples 1-7 fluctuated within 0.2% within one month of storage, and the samples were stable. Figure 2-Figure 5 The state diagram of the halquinol suspension in Examples 1-3 at 0h, 3d, 15d, and 1m. Figure 2-Figure 5 1, 2, and 3 are Example 1, Example 2, and Example 3, respectively.

[0060] Test Example 2

[0061] Viscosity test

[0062] The dynamic viscosity of the Halquinol suspensions of Examples 1-7 was tested at different temperatures using a ViscoQC 100 rotational viscometer. The test results are shown in Table 3.

[0063] Table 3 Dynamic viscosity of the Halquinol suspension of Examples 1-7 at different temperatures

[0064]

[0065] As can be seen from Table 3, the Halquinol suspensions of Examples 1-7 have better fluidity than glycerol. When the temperature is lowered to -10°C, the viscosity change value is within 20%, and still has good fluidity. Figure 6 It can be seen that the halquinol suspension of Example 3 did not show stratification when left standing at -10°C for 48 hours.

[0066] Test Example 3

[0067] Spraying uniformity test

[0068] The Halquinol suspensions of Examples 1-7 were subjected to a spraying test. Before the experiment, the Halquinol suspensions of Examples 1-7 were sprayed onto square white paper sheets multiple times, and the flatness of the paper sheets and the spraying effect were observed under ultraviolet light to determine the spraying uniformity. At the same time, the Halquinol suspensions of Examples 1-7 were sprayed onto filter paper multiple times, and after the filter paper was dried, different positions on the paper sheets were cut out, and the content of Halquinol at different positions on the paper sheets was detected by gas phase external standard to determine the spraying uniformity.

[0069] Table 4 Spraying effect of Halquinol suspension of Examples 1-7

[0070]

[0071] Figure 7 This is a test diagram of the uniformity of spraying of the Halquinol suspension in Example 3. Figure 7It can be seen from Table 4 that the spraying effect of the Halquinol suspension of Examples 1-7 is uniform, and the Halquinol components are evenly distributed.

[0072] Test Example 4

[0073] Particle size detection

[0074] The particle size of the halquinol suspensions of Examples 1-7 was measured using a laser particle size analyzer (Malvern MS2000), and the results of the 50% passing particle size D50 are shown in Table 5.

[0075] Table 5 Particle size test results of Halquinol suspension of Examples 1-7

[0076]

[0077] It can be seen from Table 5 that 50% of the particle size D50 of the Halquinol suspension is below 200 μm. The size of the Halquinol suspension prepared by the present invention is suitable for spraying with fan-shaped nozzles and centrifugal nozzles, and can be combined with a CNC breeding system for spraying.

[0078] The above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

Claims

1. A halquinol suspension, characterized in that: The halquinol suspension comprises the following raw materials calculated by mass percentage: 1% to 20% of halquinol, 0.05% to 2% of suspending agent, 1.5% to 5% of solubilizing agent, 1% to 5% of antifreeze agent, 2% to 10% of auxiliary agent, and the balance is water.

2. The halquinol suspension according to claim 1, characterized in that The halquinol comprises the following raw materials: 57% to 74% by weight of 5,7-dichloro-8-hydroxyquinoline, 23% to 40% by weight of 5-chloro-8-hydroxyquinoline and 0% to 4% by weight of 7-chloro-8-hydroxyquinoline.

3. The halquinol suspension according to claim 1 or 2, characterized in that The dynamic viscosity of the halquinol suspension is 85 to 160 mPa·s.

4. The halquinol suspension according to claim 1 or 2, characterized in that The particle size of the halquinol suspension is 100 to 200 μm.

5. The halquinol suspension according to claim 1, characterized in that The suspending agent is a polymer suspending agent; the solubilizing agent is an ionic surfactant; the antifreeze agent is a sugar antifreeze agent; and the auxiliary agent is a ternary weak acid and its derivatives.

6. The halquinol suspension according to claim 1 or 5, characterized in that The suspending agent is a cellulose suspending agent; the solubilizing agent is an anionic surfactant; the antifreeze agent is a small molecule sugar antifreeze agent; and the auxiliary agent is one or more of citric acid and sodium citrate.

7. The halquinol suspension according to claim 6, characterized in that The suspending agent is one or more of methyl cellulose, sodium carboxymethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl cellulose, and hydroxyethyl cellulose; the solubilizing agent is one or more of sodium dodecyl sulfate and sodium dodecylbenzene sulfonate; and the antifreeze agent is one or more of sucrose, lactose, maltose, and trehalose.

8. A method for preparing the halquinol suspension according to claim 1, characterized in that: The method comprises the following steps: mixing the halquinol, suspending agent, solubilizing agent, antifreeze agent and auxiliary agent in a formula amount to obtain solid powder, crushing the solid powder to obtain a dry suspension, sieving the dry suspension, stirring and mixing with a formula amount of water to obtain the dry suspension.

9. The method for preparing the halquinol suspension according to claim 8, characterized in that: The mesh number of the sieve through which the dry suspension is sieved is 100 to 200 meshes.

10. The method for preparing the halquinol suspension according to claim 8, characterized in that: The stirring speed is 200-2000 r / min; the stirring temperature is 10-30°C.

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