WO2023116026A1

WO2023116026A1 - Suspending aid, preparation method therefor and use thereof

Info

Publication number: WO2023116026A1
Application number: PCT/CN2022/115401
Authority: WO
Inventors: 谭志坚; 赵一阳; 翁亚彪; 王振兴; 刘肖娟; 袁增辉; 刘丽丹
Original assignee: 佛山市正典生物技术有限公司
Priority date: 2021-12-23
Filing date: 2022-08-29
Publication date: 2023-06-29
Also published as: CN114224833B; CN114224833A

Abstract

A suspending aid, a preparation method therefor and the use thereof. The suspending aid comprises the following components in weight percentages: 0.1%-30% of a polyacrylate monovalent salt, 0.1%-50% of a visual characteristic reagent, 0.1%-50% of a rheological property regulator and 0.1%-90% of a flowing property regulator, wherein the visual characteristic reagent is selected from a polyphosphate monovalent salt and/or an EDTA salt, the visual characteristic is that after the suspending aid is added to water, precipitation and/or turbidity are/is generated firstly, then the precipitation and/or turbidity disappear(s), and when the visual characteristic appears, it is shown that the influence of the hardness of water on the rheological property of the system is substantially eliminated, and a water medium with a required viscosity is already obtained. The suspending aid can be used for preparing aqueous suspension media of suspension vaccines, medicines, additives, etc.

Description

A kind of suspending agent and its preparation method and application

technical field

The invention belongs to the field of thickeners, and in particular, relates to a suspending agent and its preparation method, application and application method. The suspending agent is used to form a suspending water medium with water according to dosage, especially It has obvious visual characteristics when it is used for water with a hardness of 180-1000ppm to form an aqueous medium.

Background technique

Suspending agents are used in a wide range of fields, and are widely used in many industries such as food industry, coatings, biology, pharmaceutical preparations, and vaccine immunity. Suspending agent is generally a composition whose main component is dissolved in water and fully hydrated under certain conditions to form a viscous, slippery macromolecular substance, which has the functions of thickening and suspending, and is called here It is a rheology modifier (abbreviation, rheology modifier), and its dosage is generally very small, usually only a few thousandths to a few percent, but it can very effectively improve the viscosity of the water system, making it necessary to Substances suspended in water do not settle.

Sometimes it is necessary to prepare a mixture (medium) with suspension, thickening, and thixotropic functions from a solid suspending agent powder composition and water on site. This may be due to poor stability of the liquid formulation and cannot be stored for a long time , and the use time of the prepared mixture is short, so long-term stability studies are not required; or because the transportation cost of the solid suspension powder is relatively low, and the system contains a large amount of water after being formulated into a liquid. It causes a significant increase in transportation costs; or because the suspending agent is used in conjunction with other products, and other products are not suitable for long-term storage in aqueous solution, or additional costs will be incurred for storage. Therefore, many commercially available suspending agents are solid composition powders, which are prepared on site with water to suspend required materials, such as vaccines, drugs, and additives. For example, coccidia oocyst vaccines are suspended for chickens to drink to obtain immunity.

The preparation of suspending agent solution generally needs to use water, the simplest is to use tap water, or directly use ground water (such as well water, spring water, etc.). However, the water quality varies greatly in different regions, and in some mountainous areas, the water hardness is relatively high. Even tap water can vary widely in hardness, let alone untreated groundwater. Hard water is water that contains calcium and magnesium ions. The hardness of water can be graded (calculated by calcium carbonate): 1. Soft water: 0-60ppm; 2. Slightly hard water: 60-120ppm; 3. Hard water: 120-180ppm; The hardness of tap water is generally less than 450ppm. Although the hardness of water in many areas meets the national standard, the hardness is still high; and many breeding plants directly use groundwater as daily water, and many breeding farms are distributed in mountainous areas, the hardness of groundwater will be relatively high, and the water in many areas will It exceeds the standard of 450ppm, and may even reach 700ppm, and in extreme cases, it may even be as high as around 1000ppm. Hard water can be divided into temporary hardness and permanent hardness. Temporary hardness is caused by bicarbonate of calcium and magnesium, which can be reduced by boiling. Permanent hardness is caused by sulfates etc. and cannot be reduced by boiling. Although it is believed that hard water will not produce obvious harm to health, it will bring a lot of inconvenience to daily life and industrial production. For example, hard water needs to consume a lot of washing powder when washing clothes, so ordinary washing powder will add detergent.

The chemical formula of sodium polyacrylate can generally be expressed as (C ₃ H ₃ NaO ₂ ) _n , which is a common rheological property modifier and is widely used as a food additive, which has the ability to change the rheological properties of the medium (ie, thicken) , emulsification, suspending effect, also used as water treatment agent, brine refining and latex thickening. The aqueous solution of sodium polyacrylate has good suspending properties, and can be used to suspend particulate matter such as drugs, feed, vaccines, etc. Sodium polyacrylate can be dissolved in sodium hydroxide solution, but precipitates will form in aqueous solutions such as calcium hydroxide and magnesium hydroxide, for example, precipitates will form in hard water containing more divalent positive ions such as calcium ions and magnesium ions. Therefore, when sodium polyacrylate is added to hard water, due to the formation of precipitates, its thickening function will be weakened, and it will also cause different viscosities and suspension capabilities of the feed liquid prepared with the same amount of sodium polyacrylate and water with different hardness . Although this can improve the viscosity difference by adjusting the amount of sodium polyacrylate added, but this will cause poor operability. For example, general breeders do not know how much sodium polyacrylate to add to achieve the required viscosity, and it needs to be measured with a viscosity instrument, which is troublesome to operate. However, the viscosity of the aqueous suspension medium is too large to cause poor fluidity of the system, and there is no tube siphon phenomenon, resulting in greater difficulties in distribution and pouring, making even distribution very difficult. Therefore, the use of sodium polyacrylate in hard water is still a big challenge, and there is a realistic demand to obtain a feed solution with less viscosity difference in water with different hardness.

In order to solve the final suspension obtained when the suspending agent containing sodium polyacrylate is prepared with pure water (hardness less than 20ppm water), low hardness tap water and high hardness tap water, high hardness natural water (such as well water or mountain spring water) For the problem of huge difference in viscosity, one method is to use pure water to prepare, which can obtain almost completely uniform viscosity, but the purchase cost of pure water will bring a certain increase in product use cost; another method is to boil hard water Soften to obtain water with significantly reduced hardness, which can greatly reduce the difference in viscosity, but boiling can only effectively reduce the temporary hardness (mainly convert bicarbonate into insoluble carbonate through high temperature and precipitate from water to reduce the hardness of water ), and cannot effectively reduce the permanent hardness. And boiling requires energy consumption, although this has certain advantages for some occasions that require heating to provide rapid solubility, but for occasions that require room temperature water for sample preparation, the boiled water needs to be cooled before use, not only consumes Energy, but also time-consuming (such as coccidian oocyst vaccines are not resistant to high temperatures, some drugs will deteriorate at high temperatures).

Therefore, for such suspending agents that are greatly affected by water hardness, if hard water with different hardness is not specially treated, it can be directly used to prepare a suspension with the required viscosity, and the viscosity difference of the final suspension is not too small. Big, it seems very meaningful. And if there are obvious visible phenomena during the preparation process to show that the influence of the hardness of the suspending agent has been eliminated, it will be more conducive to the on-site operation.

Contents of the invention

The object of one aspect of the present invention is to provide a kind of suspending agent, and described suspending agent is used for forming the aqueous medium with water suspending property according to dosage, especially when being used for forming aqueous medium with the water hardness of 180～1000ppm. Visual characteristics, the suspending agent includes the following components in weight percentage: 0.1-30% polyacrylate monovalent salt, 0.1-50% visual characteristic reagent, 0.1-50% rheological property regulator, flow property regulator 0.1-90%, the visualization feature reagent is selected from polyphosphate monovalent salt and/or chelating agent containing amino and carboxyl groups, and the visualization feature is that after adding the suspending agent to the above water, a precipitate is first formed and/or becomes turbid, Then the precipitation and/or turbidity disappear, and when this visual feature is displayed, it indicates that the influence of water hardness on the rheological properties of the system has been basically eliminated, and the aqueous medium with the required viscosity has been obtained, wherein the above-mentioned dosage is 3-50 g of suspending agent added to 1 L of water , the viscosity of the water medium is 20mpa.s ~ 500mpa.s (rotational viscometer, 6rpm using 1 # rotor measurement).

The above-mentioned suspending agent can also be used in water with a hardness of less than 180ppm, such as pure water with a hardness of 20ppm. Although it does not show visual features, when added to pure water according to the above dosage, an aqueous medium with a desired viscosity can be obtained.

More preferably, the water has a hardness of 180 to 800 ppm, and further, the water has a hardness of 180 to 500 ppm.

More preferably, the above-mentioned dosage is 3-40 g of suspending agent added to 1 L of water, and the viscosity of the aqueous medium is 20 mpa.s to 500 mpa.s; The achieved viscosity is 20mpa.s-500mpa.s; more preferably, the above dosage is 3-20g of suspending agent added to 1L of water, and the achieved viscosity of the aqueous medium is 20mpa.s-500mpa.s.

The polyacrylic acid can refer to a polymer comprising an acrylic acid structure, which can be a homopolymer or a copolymer; preferably, the polyacrylic acid root monovalent salt is selected from sodium polyacrylate, potassium polyacrylate, lithium polyacrylate, One or more mixtures of ammonium polyacrylate.

Preferably, the polyphosphate monovalent salt is selected from one or more mixtures of sodium polyphosphate, potassium polyphosphate, lithium polyphosphate, and ammonium polyphosphate.

Preferably, the above-mentioned chelating agent containing amino and carboxyl groups is selected from EDTA salts.

Preferably, the aforementioned EDTA salt is selected from disodium EDTA and/or dipotassium EDTA and/or dilithium EDTA and/or dilithium EDTA.

Preferably, the process from the formation of precipitation and/or turbidity to the disappearance of precipitation and/or turbidity occurs within 20 minutes, and the process of adding the above suspending agent is accompanied by stirring; more preferably within 1 to 20 minutes; more preferably the above process Occurs within 3 to 10 minutes.

Preferably, the aforementioned rheology modifier is selected from alkali metal salts and/or ammonium salts.

Preferably, the above-mentioned alkali metal salt is selected from one or more mixtures of hydrochloride, sulfate, sulfite, thiosulfate, hydrobromide, hydroiodide and nitrate of alkali metal ions .

Preferably, the ammonium salt is selected from one or more of ammonium ion hydrochloride, sulfate, sulfite, thiosulfate, hydrobromide, hydroiodide and nitrate.

Preferably, the fluidity regulator is selected from one or more mixtures of fumed silica, precipitated silica, anhydrous sodium sulfate, anhydrous glucose, spherical silica, talcum powder, and mica powder.

More preferably, above-mentioned suspending agent comprises the component of following percentage by weight:

1-25% polyacrylic acid root monovalent salt, 2-40% visualization characteristic reagent, 1-40% rheological property regulator, and 5-90% fluidity property regulator.

1-25% of monovalent salt of polyacrylic acid root, 2-40% of visual characteristic reagent, 1-40% of rheological property regulator, and 5-80% of fluidity property regulator.

3-25% of monovalent polyacrylic acid root salt, 10-40% of visual characteristic reagent, 1-30% of rheological property regulator, and 40-80% of fluidity property regulator.

Sodium polyacrylate 3-25%, sodium polyphosphate and/or disodium EDTA 10-40%, sodium chloride and/or potassium chloride and/or ammonium chloride and/or sodium sulfate and/or potassium sulfate and / or ammonium sulfate and / or sodium thiosulfate and / or potassium thiosulfate and / or ammonium thiosulfate 2 ~ 25%, fumed silica and / or spherical silica 0.5 ~ 10%, the balance is none Glucose water, in which sodium polyphosphate and/or disodium EDTA are the visual characteristic reagents, the visual characteristic is that after adding suspending agent in hard water, precipitation and/or turbidity first occurs, and then the precipitation and/or turbidity disappears.

Further preferably, the above-mentioned suspending agent is used to form an aqueous medium with water having a hardness of 180-500 ppm, which consists of the following components in weight percentage:

Sodium polyacrylate 5-25%, sodium polyphosphate and/or disodium EDTA 10-25%, sodium chloride and/or potassium chloride and/or ammonium chloride and/or sodium sulfate and/or potassium sulfate and /or ammonium sulfate and/or sodium thiosulfate and/or potassium thiosulfate and/or ammonium thiosulfate 2-25%, fumed silica and/or precipitated silica and/or spherical silica 0.5～ 10%, and the balance is anhydrous glucose, wherein sodium polyphosphate and/or disodium EDTA are visual characteristic reagents, and the visual characteristic is that precipitation and/or turbidity occur first after adding suspending agent in hard water, and then precipitation and/or or the turbidity disappears.

Further preferably, the above-mentioned suspending agent is used to form an aqueous medium with water with a hardness of less than 1000 ppm, especially water with a hardness of 180 to 500 ppm, which consists of the following components in weight percentage:

Sodium polyacrylate 3-20%, sodium polyphosphate and/or disodium EDTA 20-50%, sodium chloride and/or potassium chloride and/or ammonium chloride and/or sodium sulfate and/or potassium sulfate and /or sodium thiosulfate and/or potassium thiosulfate and/or ammonium thiosulfate 2-20%, fumed silica and/or precipitated silica and/or spherical silica 0.5-10%, balance It is anhydrous glucose, wherein sodium polyphosphate and/or disodium EDTA are the visual characteristic reagents, and the visual characteristic is that after adding the suspending agent in hard water, precipitation and/or turbidity first occurs, and then the precipitation and/or turbidity disappears.

Another object of the present invention is to provide the use of the above-mentioned suspending agent in the preparation of aqueous suspensions of coccidia vaccines, medicines or additives.

Preferably, the above-mentioned coccidia vaccines are selected from coccidia oocyst vaccines.

Preferably, the above coccidiosis oocyst vaccine is selected from chicken coccidia oocyst vaccine, rabbit coccidia oocyst vaccine, pigeon coccidia oocyst vaccine, duck coccidia oocyst vaccine, porcine coccidia oocyst vaccine, bovine coccidia oocyst vaccine capsule vaccine or canine oocyst vaccine.

Another object of the present invention is to provide the preparation method of the above-mentioned suspending agent with visual characteristics that can be used in hard water. The preparation method includes first mixing part or all of the flow property modifier with polyacrylate monovalent salt, and then adding The visual characteristic reagent and the rheology modifier and the balance of the flow modifier are mixed evenly.

Another object of the present invention is to provide a method of using the above-mentioned suspending agent for hard water with visual features.

The relationship between the addition amount of the suspending agent and the ratio of the visual characteristic reagent in the formula composition and the hardness of the water that can be applied should satisfy the following relationship: the addition amount of the suspending agent × the ratio of the visual characteristic reagent in the formula composition The ratio (ie, the amount of visualization feature reagent added) is sufficient to complex the hardness-producing ions in water of the applicable hardness.

The method of use includes adding the suspending agent into the water according to the above dosage, and if there is precipitation and/or turbidity in the water, the stirring is continued for 3 to 10 minutes, and the precipitation and/or turbidity disappears, indicating that the ion of hardness in the water is paired with polyacrylic acid. The influence of the viscosity of sodium has been eliminated, and the aqueous medium with the desired viscosity has been obtained; or the method of use includes adding the suspending agent into the water according to the above dosage, and the water has precipitation and/or turbidity, and the stirring is continued for 3 to 10 minutes , the precipitation and/or turbidity did not disappear, and continued to stir for another 3 to 10 minutes. If the precipitation and/or turbidity still did not disappear, it indicated that the hardness of the water exceeded the hardness requirement that the suspending agent could be used according to the dosage, The water can be reduced in viscosity by boiling or other means, and then the above dose of suspending agent is added, and precipitation and/or turbidity occurs in the water, and the stirring is continued for 3 to 10 minutes, and the precipitation and/or the turbidity disappear, indicating The impact of the ions that produce hardness in water on the viscosity of sodium polyacrylate has been eliminated, and the aqueous medium of the required viscosity has been obtained; or the method of use includes adding the suspending agent to the water according to the dosage, and the water has precipitation and / or turbidity occurs, continue to stir for 3 to 10 minutes, the precipitation and / or turbidity does not disappear, continue to stir for another 3 to 10 minutes, the precipitation and / or the turbidity does not disappear, continue to add suspending agent, and then Continue to stir for 3 to 10 minutes. If the precipitation and/or turbidity disappears, it means that the influence of the ions that produce hardness in the water on the viscosity of sodium polyacrylate has been eliminated, and the aqueous medium with the required viscosity has been obtained. The amount added during the process does not exceed the amount added for the first time, for example, it can be 1 times, 1/2, 1/3, 1/4, etc. of the amount added for the first time; or the method of use includes adding the suspending agent according to the above dosage In the water, there is no precipitation generation, which shows that the content of ions that produce hardness in the water is relatively small, which basically has no effect on the viscosity of sodium polyacrylate, and the aqueous medium with the required viscosity has been obtained.

When the suspending agent of the present invention is added to water, it is preferably passed through a porous partition or a porous diaphragm to control the adding speed of the suspending agent.

The viscosity of the aqueous medium with the required viscosity is 20mpa.s-500mpa.s, which can meet the suspension requirements of conventional medicines, coccidia vaccines and additives. For example, for coccidia oocysts, when the viscosity of the water medium reaches 30mpa.s-150mpa.s, it has a good suspension effect.

The suspending agent of the present invention can be used for water with different hardness, and when it is used to prepare a water suspension medium with a certain viscosity, it can be clearly seen that the influence of the hardness of water on the viscosity of sodium acrylate has been eliminated, and the water medium with the required viscosity has been obtained , without measuring the viscosity. Although there is no obvious visual feature for water with lower hardness, it can still obtain the required viscosity water medium by adding it to water according to the dosage.

The suspending agent of the present invention can be used to form a viscous water medium in water with a hardness of less than 1000ppm, especially hard water with a hardness of 180-1000ppm. The water does not require additional treatment and has visual features; it is further preferably used in water with a hardness of 180-800ppm ; Further preferably used in water with a hardness of 180-500ppm.

Description of drawings

Fig. 1 is the process of preparing an aqueous suspension medium using 800ppm hard water and the suspending agent of Example 1, and obvious visual features can be seen. Wherein only hard water is not added suspending agent in the beaker on the left, after adding suspending agent in the beaker in the middle, stir for 1 minute, add suspending agent in the beaker on the right and stir for 6 minutes.

From left to right in Fig. 2 are water suspension media prepared by using pure water with hardnesses of 800ppm, 450ppm, 200ppm, and less than 20ppm respectively and the suspending agent of Comparative Example 1.

Fig. 3 is successively from left to right without adding suspending agent in 800 hard water, adding suspending agent 4g of embodiment 2, adding suspending agent 8g of embodiment 2, adding suspending agent 12g of embodiment 2 after fully stirring photo.

Detailed ways

In the description of the present invention, "multiple" means two or more.

In the suspending agent of the present invention, 1L hardness is less than the hard water of 1000ppm, especially the hard water that hardness is 180～1000ppm adds 3～50g suspending agent, the viscosity of the water suspending medium of preparation is about 20mpa.s～500mpas (rotational viscosity Meter, 6rpm using 1 # rotor measurement), can meet the suspension of conventional medicines, feed, coccidia vaccines such as coccidia oocyst vaccines. In the description of the present invention, "monovalent salt of polyacrylate" refers to the salt formed by polyacrylate ion and monovalent positive ion. The polyacrylic acid refers to a polymer containing an acrylic acid structure, which can be a homopolymer or It is a copolymer, and the polymer containing the acrylic acid structure may be acrylic acid, methacrylic acid, ethacrylic acid or a combination thereof; collectively referred to as polyacrylic acid here. The salt formed by polyacrylate ion and monovalent positive ion includes but not limited to sodium polyacrylate, potassium polyacrylate, lithium polyacrylate, ammonium polyacrylate. In the suspending agent of the present invention, polyacrylate root monovalent salt is used as a rheology modifier (or called a thickener), and its effect is that when added to water, the viscosity of water is increased and or water has a suspending effect, so that Suspend particles such as drugs, feed, and coccidia oocyst vaccines in the water. The density of particles such as drugs, feed, inactivated coccidian vaccines is generally 0.8~1.5g/cm ³ , and the water medium with a viscosity of 20mpa.s~500mpa.s can generally suspend them, meeting the general use requirements of 6~12h.

In the description of the present invention, "polyphosphate monovalent salt" refers to the salt formed by polyphosphate ion and monovalent positive ion, including but not limited to sodium polyphosphate, potassium polyphosphate, lithium polyphosphate , Ammonium polyphosphate. In the description of the present invention, "the chelating agent containing amino group and carboxyl group" means that there are multiple coordination atoms (such as O and N) in the molecule having amino group and carboxyl group at the same time, which can interact with most metal ions such as hard water such as calcium and magnesium. Multivalent ions form a stable chelate (chelate) material, such as ethylenediaminetetraacetic acid, and further preferably water-soluble substances, so the chelating agent containing amino and carboxyl groups is further preferably EDTA or its salt; "EDTA salt "Refers to the salt formed by EDTA and positive ions, including but not limited to disodium EDTA, dipotassium EDTA, dipotassium EDTA, diammonium EDTA. Polyphosphate radical monovalent salt and/or EDTA salt are used as visual characteristic reagent in the present invention, and it is added in hard water and makes suspending agent of the present invention have obvious visual characteristic, prompting operator's water hardness to thickener thickener. The influence of thickening and suspending effects has basically been eliminated, and the aqueous medium with the required viscosity has been prepared. However, this characteristic such as viscosity is allowed to fluctuate moderately in water of different hardness.

The polyphosphate monovalent salts used in the present invention, such as sodium polyphosphate, are generally condensed phosphates with different chain lengths such as dimerization and trimerization, and are easily soluble in water. They have a strong ability to chelate metal ions, especially calcium and magnesium ions, so they can be used as water softeners. The inventors of the present application have found that when polyphosphate (such as sodium tripolyphosphate) and sodium polyacrylate are added to hard water together, there is a phenomenon: earlier in the water, precipitation is generated (water becomes turbid), and after stirring for a period of time, the precipitation disappears (water becomes turbid). change to clarify). For the effect of sodium polyphosphate and calcium plasma in hard water, Qin Anrong (properties and uses of sodium polyphosphate [J]. Yunnan Chemical Industry, 1990, (3): 34-37) has carried out detailed description, its reaction formula Can be expressed as:

2Na ₅ P ₃ O ₁₀ +5Ca ²⁺ ＝Ca ₅ (P ₃ O ₁₀ ) ₂ +10Na ⁺

Ca ₅ (P ₃ O ₁₀ ) ₂ +3Na ₅ P ₃ O ₁₀ ＝5Na ₃ CaP ₃ O ₁₀

The resulting polyphosphate containing calcium and sodium is soluble in water, which is why sodium polyphosphate can soften hard water.

When sodium polyacrylate is added to hard water, polyacrylate ions will combine with divalent calcium and magnesium in hard water to form a white precipitate, and the speed is relatively fast. Sodium polyacrylate and sodium polyphosphate were added to hard water together, and it was found that flocculent precipitates were formed in the water (the water became turbid), and after stirring for a period of time, the precipitation and turbidity disappeared (the water became transparent again). The reason may be that polyacrylic acid ion reacts with calcium and magnesium ions to form calcium polyacrylate, and its reaction is fast, while calcium polyacrylate is precipitated in water, so when sodium polyphosphate and sodium polyacrylate are added together, calcium polyacrylate will be formed first. Precipitation; in the process of continuing to stir, the polyphosphate ion captures the calcium in the calcium polyacrylate or the magnesium in the magnesium polyacrylate, although the speed is relatively slow, but the complexation ability is very strong. With the combination of phosphate ions, the calcium polyacrylate and magnesium polyacrylate formed in the early stage gradually decompose, and sodium polyacrylate is formed in the system, and the precipitate disappears.

During this process, white precipitates begin to form, indicating that the content of calcium and magnesium ions in the water is relatively high, and the hardness of the water is relatively high. Then the white precipitate disappears and the solution becomes transparent, indicating that the calcium and magnesium ions in the hard water have been basically complexed by sodium polyphosphate, and the influence of water hardness on sodium polyacrylate has been basically eliminated.

In addition to sodium polyphosphate, other complexing agents can also play a similar role, such as bidentate or multidentate ligands, such as chelating agents containing amino and carboxyl groups. Chelating agents containing amino and carboxyl groups can be selected from EDTA or its sodium salt, potassium salt and other soluble salts. For example, disodium EDTA can be used as a complexing agent to form soluble complexes with calcium and magnesium ions to reduce free calcium in the water system , Magnesium ion content. Its calcium ion complex is shown in formula (I):

And the complex is soluble in water.

When the system contains polyacrylate monovalent salts such as sodium polyacrylate and disodium EDTA and other aminocarboxyl chelating agents, there will also be precipitation/turbidity first, and then the precipitation/turbidity disappears, which is used as a visual feature Preparation of suspensions.

The present invention selects polyacrylic acid radical monovalent salt, polyphosphate radical monovalent salt and EDTA sodium, potassium salt, because monovalent salt can affect the viscosity that polyacrylic acid ion hydration produces, and this is different from divalent ions such as calcium , monovalent ions such as sodium and potassium will reduce the viscosity produced by hydration, but will not cause precipitation.

The viscosity produced by hydration of polyacrylate ions is affected by monovalent ions. With the increase of the amount of monovalent ions added, the viscosity produced by hydration gradually decreases. When the suspending agent mixture containing sodium polyacrylate is added into water, the viscosity of the water system is related to the concentration of polyacrylate ions on the one hand, and also related to the monovalent positive ions (mainly sodium, potassium ions) in the water system on the other hand. ), divalent positive ions (mainly calcium, magnesium ions) content. The concentration of polyacrylate ions is positively correlated with the viscosity of the water system, the greater the concentration of polyacrylate ions, the greater the viscosity of the water system, and vice versa, but the relationship is not linear. The concentration of monovalent positive ions is negatively correlated with the viscosity of the water system. When the concentration of polyacrylic acid ions remains constant, the greater the concentration of monovalent positive ions, the smaller the viscosity of the water system, but its influence increases with a The increase of valence ions gradually decreases (also a nonlinear relationship) (relevant relationship can refer to the literature: Research on the viscosity behavior of polyacrylate sodium synthesized by irradiation method, Zhao xin, Huang haibo, Cui Jianchun, Li Cui, Journal of Xinjiang University ( Natural Science Edition). 1993, 10(03):60-62, Table 3 and Figure 1 published on page 62), but no precipitate was formed. Since divalent positive ions or multivalent positive ions can form precipitation with polyacrylic acid ions, polyacrylic acid ions cannot exert their thickening effect. When the mixture containing polyacrylate monovalent salt and polyphosphorus monovalent salt and/or EDTA monovalent salt is added to water, polyphosphate ion and/or EDTA chelate with calcium and magnesium ions to eliminate calcium and magnesium The effect of ions on the concentration of polyacrylic acid ions, while releasing monovalent ions. When the hardness of hard water is high, it is necessary to add more polyphosphate and/or EDTA to make the precipitation of the system disappear (that is, to complex the calcium and magnesium ions in the water), but at the same time, the system will also release more monovalent ions . Although in this process, the viscosity of the system has a tendency to increase due to the addition of more suspending agents to cause the concentration of polyacrylic acid radical ions in the system to increase, but because more polyphosphate radical monovalent salts and/or The monovalent positive ions released by the EDTA salt reduce the viscosity of the system. Therefore, the viscosity of the final aqueous medium is kept within a certain range.

Since the viscosity of polyacrylic acid ion hydration is affected by monovalent ions, adding a certain amount of monovalent ion salts to the system can further reduce the difference in viscosity. Therefore, a rheology modifier is also added to the suspending agent of the present invention to adjust the viscosity of the final aqueous medium, so as to maintain it within a certain range. When the suspending agent of the present invention is added to water, along with the white precipitate disappears, the calcium and magnesium ions in hard water have been basically complexed by polyphosphate ions, and the influence of calcium and magnesium ions on the viscosity produced by the hydration of polyacrylic acid ions It has been basically eliminated that the viscosity of water is only affected by the concentration of polyacrylate ions and the concentration of monovalent ions. The inventor of the present application finds that within the ratio range of the limited suspending agent of the present invention and hard water (need to add 3～50g in 1L water, more preferably 3～40g, further preferably 3～30g, more preferably 3 ~20g suspending agent), the final viscosity of the water system can be maintained at 20mpas ~ 500mpas, which can meet the suspension requirements of conventional drugs, feed, coccidia oocyst vaccines and other particles, especially for coccidia oocyst vaccines. suspension requirements. Therefore, after adding the suspending agent in hard water, the phenomenon that a precipitate is first formed, and then the precipitate disappears can be used as a visual feature, which can be conveniently used as a sign of the state of the preparation process.

Therefore, in the suspending agent of the present invention, the visual characteristics are related to the hardness of water on the one hand, and polyacrylic acid ion on the other hand, or the common effect of various components. Viscosity characteristics are related to polyacrylate ion, also related to visual characteristic agent, and also related to rheological performance modifier, which is the result of the interaction of various components.

The rheology modifier described in the present invention is used to adjust the viscosity of the water system containing specific polyacrylic acid ion concentration. As mentioned above, sodium ions, potassium ions, lithium ions, and ammonium ions can adjust the viscosity of water systems containing polyacrylate ions at different concentrations. The purpose of adding the rheological property regulator in the present invention is to obtain relatively small differences in rheological properties of water with different hardnesses under the premise of sacrificing certain rheological properties (such as viscosity). Therefore, the rheology modifier of the present invention includes but is not limited to alkali metal salts or ammonium salts, for example, salts of monovalent positive ions such as sodium salts, potassium salts, lithium salts, ammonium salts, or mixtures thereof. Said salts may be hydrochlorides, sulfates, sulfites, thiosulfates, hydrobromides, hydroiodides, nitrates.

Specifically, the rheology modifiers of the present invention include but are not limited to sodium chloride, potassium chloride, lithium chloride, ammonium chloride; sodium sulfate, potassium phosphate, lithium sulfate, ammonium sulfate; sodium sulfite, potassium sulfite, Lithium sulfite, ammonium sulfite; sodium thiosulfate, potassium thiophosphate, lithium thiosulfate, ammonium thiosulfate; sodium bromide, potassium bromide, lithium bromide, ammonium bromide; sodium iodide, potassium iodide, iodide Lithium, Ammonium Iodide; Sodium Nitrate, Potassium Nitrate, Lithium Nitrate, Ammonium Nitrate or mixtures thereof.

According to the nature of sodium polyacrylate, if a large amount of this substance is added to water at one time, even if various additives are added, it will still cause the powder to agglomerate when it encounters water. The sodium polyacrylate in the agglomerate is not easy to hydrate, which will cause the A longer stirring time is required to obtain a fully hydrated and uniform feed solution. Therefore, it is an effective way to quickly obtain the feed liquid of the required suspension performance by adding it into the stirred water under the situation of controlling the speed through a porous plate or a porous membrane (in order to realize this mode, the suspending agent can be packaged in a bottle with an aluminum foil seal, Prick holes on site during use, and pour out from it [utility model patent application, patent number: ZL202122759893.6]). In order to make the suspending agent flow out from the porous plate or porous membrane smoothly, the suspending agent needs to have good fluidity, so the suspending agent of the present invention is also added with a fluidity regulator to make it have good fluidity. Otherwise, it will be difficult for the powder to pass through the small holes of the porous plate or membrane, which will make it difficult to pour the powder out. The fluidity of the fluidity modifier improves the fluidity of the suspending agent by preventing the suspending agent from absorbing moisture or having better fluidity itself. The function of the fluidity regulator in the suspending agent of the present invention is to prevent the suspending agent from being damp and agglomerated during preparation, storage and preparation, and unable to mix with water evenly. Because suspending agents generally require slow addition, pouring from porous materials is preferred. Because when a large amount of suspending agent is added to the water at one time, the surface molecules of the agglomerated sodium polyacrylate rapidly hydrate with water, resulting in the inability of the molecules inside to hydrate with water and form "fish eyes". And if the suspending agent absorbs moisture, forms small particles or becomes poor in fluidity, it is easy to block the pores. Therefore, it is necessary to add moisture-proof substances to reduce the agglomeration caused by moisture. Therefore, it is necessary to add a fluidity modifier in the suspending agent of the present invention.

The fluidity modifiers of the present invention include, but are not limited to, fumed silica, precipitated silica, anhydrous sodium sulfate, anhydrous glucose, spherical silica, talcum powder, and mica powder.

The fumed silica preferably has a primary particle size of 7-40 nm, an aggregate particle size of about 200-500 nm, and a specific surface area of 100-400 m ² /g. The untreated fumed silica aggregates contain a variety of silanol groups, which can well adjust the fluidity of moisture-absorbing components. However, fumed silica is insoluble in water, and only dispersed into the system, making the system slightly turbid and reducing a certain degree of transparency, but it is obviously different from precipitation such as calcium polyacrylate (the opacity caused by precipitation such as calcium polyacrylate is similar to that in Figure 1 The beaker in the middle, the first and second beakers on the left in Figure 2, the second beaker on the left in Figure 3, and the fumed silica is slightly turbid caused by tiny particles, as shown in the beaker on the right in Figure 1, and the right beaker in Figure 2 The first beaker, the first beaker on the right in Figure 3), so the slight turbidity caused by fumed silica does not affect the judgment of the above-mentioned visual features, and a small amount of fumed silicon can satisfy the fluidity of the powder and control the absorption Moisture is the purpose. Further, the fumed silica is preferably untreated fumed silica with better hydrophilicity.

Precipitated silica is also a commonly used fluidity regulator, but its particle size is larger than that of the gas phase method, and its primary particle size is generally below 0.3 μm. Therefore, the precipitation method required to obtain similar moisture absorption performance is relatively small. Larger, so it is easier to sink to the bottom than fumed silica in the prepared water system, so it is generally better for systems with higher viscosity. And adding it will also slightly affect this transparent state, but generally it will not affect the judgment of its "transparent" state.

Spherical silica, especially hollow spherical silica, is widely used in the powder cosmetics industry. It can be used as a component of powder cake to improve the spreadability of powder, but it is rarely used as a thickener. Hollow spherical silica is composed of nanoparticles, with a size ranging from nanometers to micrometers, and a multi-scale and multi-level nanostructure with hollow cavities. Compared with corresponding bulk materials, it has larger specific surface area, lower density, special mechanical, optical, electrical and other physical properties and application value, which has aroused great interest of scientific researchers. The spherical material determines its easy flow characteristics, which makes the prepared powder easy to flow and reduces the angle of repose of the powder. In addition, because of the large hollow ratio of hollow silica, the apparent density of hollow silica is closer to that of precipitated silica than to the density of the rest of the materials, making it easier to obtain uniform mixing, so in the present invention it is preferred.

Anhydrous sodium sulfate or anhydrous dextrose itself has low water content, which can control the hygroscopicity and fluidity of the suspension, and can be used as an electrolyte or a nutritional component. On the one hand, anhydrous sodium sulfate can be used as a monovalent alkali metal salt as a rheological property regulator, and on the other hand, it can also be used as a fluidity property regulator when there is a large amount.

During the use of the suspending agent of the present invention, if the suspending agent is added into water under stirring according to a prescribed dose, a precipitate will form, continue to stir for 3 to 10 minutes, the precipitate does not disappear, and then stir for 3 to 10 minutes, the precipitate still remains If it does not disappear, it means that the hardness of the water used is too high, which may have exceeded 1000ppm (or the hardness range defined by the formula). In this case, it is still possible to continue adding suspending agent until the feed liquid becomes transparent again, and the required viscosity can be obtained, but it is possible that the viscosity obtained by increasing the amount to obtain a transparent state is higher than that of water with normal hardness. The viscosity will be slightly higher, but it is still generally satisfactory for use. For systems with too high hardness (such as hardness exceeding 1000ppm), although this method of increasing the amount of suspending agent can generally obtain the required viscosity, this method is not very economical. Can choose to adopt boiled water to remove temporary hardness for this situation, use after cooling, perhaps adopt the method for first reducing water hardness before adding suspending agent of the present invention after all the other ways. Although the hardness of water varies greatly from place to place, there are only a few regions with a hardness exceeding 1000ppm. Therefore, the hardness of the suspending agent of the present invention for hard water is 180-1000ppm, which can meet the needs of most regions.

Below in conjunction with specific embodiment, further illustrate the present invention. The specific embodiments are carried out on the premise of the technical solutions of the present invention, and detailed implementation methods and operation processes are given. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. The experimental methods that do not indicate specific conditions in the following examples are usually carried out according to conventional conditions. Ratios and percentages are by weight unless otherwise indicated.

For viscosity testing, use a rotational viscometer [NDJ-1 rotational viscometer, Shanghai Yueping Scientific Instrument Co., Ltd.] to carry out viscosity testing at various rotational speeds.

Example 1

The composition of the suspending agent is shown in Table 1.

Table 1. Composition of Suspending Agent

聚丙烯酸钠Sodium polyacrylate	氯化钠Sodium chloride	气相二氧化硅fumed silica	无水葡萄糖anhydrous glucose	多聚磷酸钠sodium polyphosphate
9.3％9.3%	7.0％7.0%	0.9％0.9%	49.5％49.5%	33.3％33.3%

Preparation process: first mix sodium polyacrylate and fumed silica, then add sodium chloride, sodium polyphosphate and anhydrous glucose and mix well.

Method of use: Add 12g of the above suspending agent through a porous plate into 1L of stirred water with different hardness, the hardness is 800ppm, 450ppm, 200ppm, <20ppm respectively. For 800ppm hard water, when starting to add water, a large amount of flocculent precipitates are formed in the water, and the system becomes turbid. After stirring for about 3-4 minutes, the precipitation in water disappears; the feed liquid gradually becomes transparent; for 450ppm hard water, when starting to add water, there are Precipitation is formed and disappears gradually after stirring; when 200ppm hard water is added, it is slightly turbid, but the system becomes transparent soon; for pure water, except for a small amount of particles when adding, no precipitation or turbidity is seen; in this suspending agent When the formula is added to water according to the dosage, the amount of sodium polyphosphate added is the amount of calcium and magnesium ions that can be completely complexed in 800ppm hard water to meet the stated amount.

The viscosity of the water was measured after stirring. The results are shown in Table 2.

Table 2. Viscosities of prepared aqueous media

As can be seen from the above data, adding the suspending agent composition of the same weight in water of different hardnesses has the largest viscosity in purified water and the smallest in 800ppm hardness water, indicating that with the increase of water hardness, the viscosity of the aqueous solution of the suspending agent is reduced. Decrease, but for the viscosity of water with 200ppm hardness and 800ppm hardness, there is a difference of 17mpa.s at 6rpm, and a difference of 4.9mpa.s at 60rpm. Viscosity requirements ranging from 200ppm to 800ppm in hardness.

It has obvious visual features in the preparation process.

From the three pictures in Fig. 1 (from left to right are respectively 800ppm hard water, hard water with suspending agent added for 1 minute, and hard water after adding said suspending agent and stirring for 6 minutes), it can be seen that hard water itself is clear and transparent. After the suspending agent, because the polyacrylic acid ion reacts with calcium and magnesium ions to form a precipitate, the precipitate disappears and gradually becomes clear with the action of polyphosphate ion and calcium and magnesium ions, indicating that the calcium and magnesium ions in hard water have a negative effect on the water. The influence of sodium polyacrylate has been basically eliminated. The clarity of the hard water after adding the above suspending agent and stirring for 6 minutes is slightly lower than that of the hard water without adding the suspending agent (Fig. 1, left figure). The transparency is reduced; on the other hand, a small amount of air bubbles are not easy to discharge, which also causes this slightly incomplete transparent state, but the canonical characters behind are clearly visible. Regardless, the transition from a turbid state with precipitate formation to a substantially clear (transparent) state where the precipitate disappears is a visual feature.

This viscosity can fully meet the suspension requirements of oocyst vaccines. The determination process and results of suspended oocysts are as follows:

The specific operation is as follows: 15.5 mL (3090 feathers) of chicken coccidiosis quadrivalent live vaccine, batch number: 21080401, is added to 1 L of the suspension prepared above. Samples were taken from 0~0.5h, 2h, 4h, 5.5h~6h of dissolution. Sampling location: For each suspension sample, take the uppermost liquid level of the suspension (mark the upper layer), the position of the 600mL scale line of the 1L beaker (mark the middle layer), and the position of the 200mL scale line of the 1L beaker (mark the lower layer); Take 4 points on each surface, each sampling point is 1mL, and mix them as the sample of this liquid surface. Each sample was packed into a 20mL polyethylene bottle, labeled, and stoppered for inspection. Microscopic examination and counting: Take 10 μL of the above samples and place them on glass slides, and count the number of oocysts under a microscope at 10×10 times. The results are shown in Table 3

Table 3 oocyst count results (unit: piece)

It can be seen from the above data that for suspension media prepared with water of different hardness, the number of oocysts tested at different times and at different locations can be considered to have no significant difference within the error range, that is, it can completely meet the requirement of at least 6 hours for suspending oocysts. requirements (generally drinking water containing oocyst vaccines should be drunk within 6 hours).

Comparative Example 1

Referring to Example 1, the difference is that sodium chloride and sodium polyphosphate are not used, but only sodium polyacrylate, fumed silicon and anhydrous glucose are used. The original amount of sodium chloride and sodium polyphosphate is supplemented by anhydrous glucose.

Table 4 Suspending agent composition

聚丙烯酸钠Sodium polyacrylate	氯化钠Sodium chloride	气相二氧化硅fumed silica	无水葡萄糖anhydrous glucose	多聚磷酸钠sodium polyphosphate
9.3％9.3%	————	0.9％0.9%	89.8％89.8%	————

Preparation process: first mix sodium polyacrylate and fumed silicon dioxide, then add anhydrous glucose and mix well.

Use process: Add 12g of the above suspending agent through a porous plate into 1L of stirred water with different hardness, the hardness is 800ppm, 450ppm, 200ppm, and less than 20ppm. For 800ppm hard water, there will be flocculent precipitation and turbidity, which cannot be eliminated; for 450ppm hard water, there will be slight turbidity, but there is no flocculent precipitation, and it cannot be eliminated; for 200ppm water and pure water (hardness less than 20ppm), when adding and stirring, Basically no flocculent precipitation and turbidity can be seen. The slight opacity after the preparation of pure water is due to the influence of fumed silica in the suspending agent added to the system, but this is obviously different from the turbidity of 800ppm and 450ppm hard water. The phenomenon is shown in Figure 2.

The viscosity of the above-mentioned water with different hardness was measured, and the viscosity test results are shown in Table 5.

Table 5. Viscosity of preparation media

It can be seen from the above table that sodium polyacrylate has the highest viscosity in pure water. Although the state is similar to the transparency of pure water in 200ppm tap water, the viscosity is already significantly lower than the value of pure water; for 450ppm hard water, its viscosity Further decline, it is very low for 800ppm, especially the viscosity at 60rpm is very low; according to the above formula and dosage, the viscosity at 6rpm of pure water is 11.8 times that of 800ppm hard water, and the viscosity at 200ppm is 100% of that at 800ppm hard water 6.8 times; the viscosity under 200 self-water is 4.8 times of the viscosity under 450 hard water; the value corresponding to the result of Example 1 is then 1.34 (pure water and 800 hard water), 1.21 (200 tap water and 800 hard water), 1.15 ( 200 tap water vs. 450 hard water).

Comparative Example 2

Table 6. Composition of Suspending Agents

聚丙烯酸钠Sodium polyacrylate	氯化钠Sodium chloride	气相二氧化硅fumed silica	无葡萄糖no glucose	多聚磷酸钠sodium polyphosphate
9.3％9.3%	7.0％7.0%	0.9％0.9%	82.8％82.8%	————

Preparation process: first mix sodium polyacrylate and fumed silicon dioxide, then add sodium chloride and anhydrous glucose and mix well.

12g of the above suspending agent was added through a porous plate into 1L of stirred water with different hardnesses, the hardnesses being 800ppm, 450ppm, 200ppm and less than 20ppm respectively.

The viscosity of the above-mentioned water with different hardness was measured, and the viscosity test results are shown in Table 7.

Table 7. Viscosity of Prepared Water Medium

It can be seen from the above table that without adding sodium polyphosphate and only adding monovalent salt sodium chloride, its viscosity will decrease compared with that of the comparative implementation 1, which is very obvious for pure water; it will not change much for 800ppm hard water. The net result is that the difference in viscosity between different water qualities is reduced.

In comparative example 2, the viscosity under pure water 6rpm is 3.31 times of the viscosity under 800ppm hard water, and the viscosity under 200ppm is 2.37 times of the viscosity under 800ppm hard water; the viscosity under 200 self-water is 1.9 times of the viscosity under 450 hard water; Smaller than the ratio corresponding to Comparative Implementation 1 (11.8 times, 6.8 times, 4.8 times); but larger than the corresponding ratio of Example 1 (1.34 times, 1.21 times, 1.15 times).

For the suspending agent that simply adds sodium chloride, the precipitation and turbidity in hard water have no obvious change.

Comparative Example 3

Table 8. Composition of Suspending Agents

聚丙烯酸钠Sodium polyacrylate	氯化钠Sodium chloride	气相二氧化硅fumed silica	多聚磷酸钠sodium polyphosphate	无葡萄糖no glucose
9.3％9.3%	————	0.9％0.9%	33.3％33.3%	56.5％56.5%

Preparation process: first mix sodium polyacrylate and fumed silicon dioxide, then add sodium polyphosphate and anhydrous glucose and mix well.

Add 12g of the above suspending agent through a porous plate into 1L of stirred water with different hardness, the hardness is 800ppm, 450ppm, 200ppm, <20ppm respectively.

The viscosity of the above-mentioned water with different hardness was measured, and the viscosity test results are shown in Table 9.

Table 9. Viscosity of Prepared Water Medium

It can be seen from the above table that adding sodium polyphosphate can eliminate the final precipitation and turbidity problems of the system, but the viscosity difference of the system is still relatively large. In comparative example 3, the viscosity under 6rpm of pure water is 1.88 times of the viscosity under 800ppm hard water, the viscosity under 200ppm is 1.37 times of the viscosity under 800ppm hard water; the viscosity under 200 self-water is 1.17 times of the viscosity under 450 hard water .

As can be seen from Example 1 and Comparative Examples 1, 2, and 3, sodium polyphosphate and sodium chloride in the system are all indispensable parts of the formula, and they work together to realize the visual characteristics and viscosity in different hard water. Effects such as minor differences.

Example 2

For the formula of embodiment 1, in the hard water of 800ppm, adopt multiple additions, observe its phenomenon and viscosity.

Table 10. Composition of Suspending Agents

聚丙烯酸钠Sodium polyacrylate	氯化钠Sodium chloride	气相二氧化硅fumed silica	无水葡萄糖anhydrous glucose	多聚磷酸钠sodium polyphosphate
9.3％9.3%	7.0％7.0%	0.8％0.8%	54.2％54.2%	33.3％33.3%

Preparation process: After mixing sodium polyacrylate and fumed silica, add sodium chloride, sodium polyphosphate and anhydrous glucose and mix well.

Use process: add 4g to 1L water each time, add the above suspending agent three times, and stir for at least 15 minutes after each addition.

Table 11. Viscosities of formulated media

The above phenomenon can be seen in the four pictures in Figure 3 (from left to right are the photos of 800 hard water without suspending agent, adding 4g suspending agent, adding 8g suspending agent, and adding 12g suspending agent after fully stirring) See clearly. It can be seen from the above pictures that when 4g of suspending agent is added, a large amount of flocculent precipitates are formed, which should be the precipitates formed by polyacrylic acid ions encountering calcium ions, and the amount of polyphosphate ions added at this time is not enough , cannot completely complex calcium and magnesium ions, so precipitation occurs, and the blue writing on the back is completely invisible; when adding 4g of suspending agent (total 8g), with the increase of the amount added, calcium and magnesium ions are gradually complexed Combined, the precipitation gradually decreases, and the blue writing on the back is faintly visible; then add 4g of suspending agent (12g in total), the calcium, magnesium and other ions are fully complexed, and the calcium, magnesium and other ions in the precipitate generated by sodium polyacrylate and calcium, magnesium, etc. Magnesium plasma is complexed by polyphosphate ions, and the transparency increases; compared with the water before the addition, the transparency is slightly lower because the system contains a small amount of gas silicon, which affects a certain degree of transparency. It is almost transparent when it is opaque to 12g, and it has obvious visual characteristics. If 12g is added at one time, it will appear turbid at the beginning, and then become transparent as the stirring progresses, which can be used as a sign that calcium and magnesium ions have been complexed. The viscosity value is slightly different, which is related to a small amount of error in weighing and measuring.

It can also be seen from the above data that for specific hard water, when the added suspending dose is not enough, the amount of polyphosphate ions in it is not enough to complex calcium and magnesium ions in hard water, and the viscosity is obviously very low; When the amount added can fully complex calcium, magnesium and other ions in hard water, the viscosity will increase significantly.

Example 3:

The composition of the suspending agent is shown in Table 12.

Table 12. Composition of Suspending Agents

Sodium polyacrylate

Anhydrous Sodium Sulfate

fumed silica

anhydrous glucose

sodium polyphosphate

11.3%

7.5%

1.2%

50%

30%

Preparation process: After mixing sodium polyacrylate and fumed silica, add anhydrous sodium sulfate, sodium polyphosphate and anhydrous glucose and mix well.

Use process: Add 50g of the above suspending agent through a porous plate into 6L of stirred water with different hardness, the hardness is 800ppm, 450ppm, 200ppm, <20ppm respectively. For 800ppm and 450ppm hard water, there are flocculent precipitates in the water at the beginning of adding, and the system is turbid, and the precipitation in the water disappears after stirring for about 2-8 minutes; for 200ppm hard water, it is slightly turbid at the beginning of adding, but disappears soon; for pure water No white turbidity. After stirring, the viscosity of the system was measured. The results are shown in Table 13.

Table 13. Viscosities of formulated aqueous media.

As can be seen from the above data, after adding the suspending agent of the present invention, although the viscosity of general tap water and water with high hardness is different, the difference is small. The viscosity ratio of 200 tap water to 800 hard water at 6rpm is 1.13; the ratio of pure water to 800ppm hard water is 1.26.

Example 4

The above-mentioned examples are formulated according to the requirement that the viscosity of water with a hardness of about 200-800 differs little, and the sodium polyphosphate added according to the stated amount is enough to handle 800ppm hard water and produce the required viscosity feature. Considering the price of specific raw materials and the actual use situation, for the occasion of using tap water, the hardness of the water is generally less than 450ppm, according to the requirements of general tap water, to meet the formula of 200-450ppm with little difference in hardness and viscosity.

The composition of the suspending agent is shown in Table 14.

Table 14. Composition of Suspending Agents

聚丙烯酸钠Sodium polyacrylate	氯化钾potassium chloride	气相二氧化硅fumed silica	多聚磷酸钠sodium polyphosphate	无葡萄糖no glucose
12.0％12.0%	9％9%	1.2％1.2%	15.0％15.0%	62.8％62.8%

Preparation process: mix sodium polyacrylate with fumed silicon dioxide, then add potassium chloride, sodium polyphosphate, and anhydrous glucose and mix well.

Use: Add 50g of the above suspending agent through a porous plate into 6L of stirred water with different hardness, the hardness is 800ppm, 450ppm, 200ppm, <20ppm respectively. In this formulation, the amount added is the amount that can complex 450ppm hard water. In 800ppm hard water, add the above amount of suspending agent, and the lower layer of the obtained material liquid has white flocculent precipitates. After stirring for more than 20 minutes, it still cannot become transparent, indicating that the addition amount according to the above amount is not suitable for hard water with a hardness exceeding 800ppm; Take another 800ppm hard water, first add 50g of the above suspending agent and continue stirring for more than 20 minutes, the flocculent precipitation does not disappear, then add 50g of the above suspending agent and continue stirring for more than 10 minutes, and the flocculent disappears; for 450ppm hard water, when starting to add Precipitation is formed in the water, and the system is turbid, which becomes transparent after stirring for about 3-5 minutes; for 200ppm tap water, it is slightly turbid when added, but the precipitate disappears quickly; for pure water, it becomes clear after stirring. After stirring, the viscosity of the system was measured. The results are shown in Table 15.

Table 15. Viscosities of Prepared Aqueous Media

Note: Hard water ¹ is 800ppm hard water with 50g of the above suspending agent added, and hard water ² is 800ppm hard water with 100g of the above suspending agent added.

The amount that adds sodium polyphosphate in this system is less, when adding according to described dosage (50g suspending agent joins in 6L water), the amount of polyphosphate ion wherein can be the calcium, magnesium in the hard water of 450ppm hardness The plasma is all complexed. The results show that the viscosity difference for water with hardness less than 450ppm is small, and transparent material liquid can be obtained, but for water with hardness exceeding 450ppm, according to the dosage, the added polyphosphate ion is not enough to produce hardness in hard water All the ions are complexed, so flocculent precipitation occurs. When the above dosage of suspending agent is added, the viscosity of 450ppm hard water has little difference from that of 200ppm hard water, and also has little difference from that of pure water. The suspending agent can meet the requirements of using tap water to prepare an aqueous suspension with the desired viscosity.

If the formulation does not make the system clear according to the stated dose, it means that the water hardness is higher than the water hardness range used for the suspending agent. For high hardness water, the water suspension of required viscosity can be obtained by further adding suspending agent. From the results of the viscosity of hard water ² , it can be seen that when adding 100g of suspending agent to make the system just clear, the viscosity of the system is significantly higher than that of adding 50g, which is close to the viscosity of 200ppm hard water.

Example 5

The composition of the suspending agent using disodium EDTA as the visualization feature reagent is shown in Table 16.

The composition of table 16 suspending agent

聚丙烯酸钠Sodium polyacrylate	氯化钠Sodium chloride	气相二氧化硅fumed silica	EDTA二钠Disodium EDTA	无葡萄糖no glucose
7.2％7.2%	3.0％3.0%	0.7％0.7%	15％15%	74.1％74.1%

Preparation process: After mixing sodium polyacrylate and fumed silica, add sodium chloride, disodium EDTA, and anhydrous glucose and mix well.

Use: Add 100g of the above suspending agent through a porous plate into 6L of stirred water with different hardness, the hardness is 800ppm, 450ppm, 200ppm, <20ppm respectively. For 800ppm, there is a process of first becoming turbid and then clear (transparent); for 450ppm hard water, it is slightly opaque, and the system becomes transparent quickly after stirring; 200ppm tap water and pure water quickly become clear; measure the viscosity of the system after stirring; measure the system after stirring viscosity. The results are shown in Table 17.

Table 17. Viscosities of formulated media

Adding disodium EDTA to the system as a visualization reagent can also observe the change from turbidity to clarity, but it is not as obvious as using sodium polyphosphate. It may be that disodium EDTA interacts with calcium and magnesium ions faster, making the generated The calcium and magnesium ions in the calcium and magnesium polyacrylate precipitates are quickly taken away, resulting in less obvious turbidity. According to the dosage, the addition of disodium EDTA can realize the complete complexation of calcium and magnesium ions in 800ppm hard water. As a result, for 200ppm-800ppm water as a whole, a viscosity with little difference can be obtained.

Example 6

The composition of the suspending agent is shown in Table 18.

Table 18. Composition of Suspending Agents

聚丙烯酸钾Potassium polyacrylate	硫代硫酸钠Sodium thiosulfate	球形二氧化硅Spherical silica	无水葡萄糖anhydrous glucose	多聚磷酸钠/ETDA ₂Na Sodium Polyphosphate/ETDA ₂ Na
2.1％2.1%	1.8％1.8%	0.3％0.3%	87.8％87.8%	5％/3％5%/3%

Preparation process: first mix potassium polyacrylate with spherical silica, then add sodium thiosulfate, sodium polyphosphate, and anhydrous glucose and mix well.

How to use: Add 50g of the above suspending agent through a porous plate into 1L of stirred water with different hardness, the hardness is 800ppm, 450ppm, 200ppm, <20ppm respectively. Phenomenon is similar to comparative example 1: for 800ppm hard water, when beginning to add water, there is a large amount of flocculent precipitation to generate in water, and system becomes turbid, along with adding the adding of suspending agent, flocculent sedimentation reduces gradually, till last feed liquid gradually changes Transparent; for 450ppm hard water, when the water was first added, there was precipitation in the water, which gradually disappeared after stirring; for 200ppm hard water, it was slightly turbid when it was added, but the system soon became transparent; pure water did not see precipitation or turbidity; When the suspending agent is added to water, because sodium polyacrylate, etc. are diluted by more anhydrous glucose, they can be quickly hydrated when added to water, and it is easier to obtain an aqueous medium with a stable viscosity; when the suspending agent is added to water according to the stated dosage , The amount of sodium polyphosphate added can completely complex the calcium and magnesium ions in 800ppm hard water.

The viscosity of the water was measured after stirring. The results are shown in Table 19.

Table 19. Viscosities of Prepared Aqueous Media

Example 7

The composition of the suspending agent is shown in Table 20.

Table 20. Composition of Suspending Agents

聚丙烯酸钾Potassium polyacrylate	氯化铵ammonium chloride	球形二氧化硅Spherical silica	无水葡萄糖anhydrous glucose	多聚磷酸钠sodium polyphosphate
9.5％9.5%	6.0％6.0%	0.9％0.9%	48.3％48.3%	35.3％35.3%

Preparation process: first mix potassium polyacrylate with spherical silica, then add ammonium chloride, sodium polyphosphate, and anhydrous glucose and mix well.

Usage method: under stirring, add 12g of the above suspending agent into 1L of water with different hardness through a porous plate, the hardness is 800ppm, 450ppm, 200ppm, <20ppm respectively. Observed phenomenon is similar to comparative example 1: for 800ppm hard water, when beginning to add suspending agent, there is a large amount of flocculent precipitates to generate in the water, and system becomes turbid, and precipitation disappears in continuing to stir, and system becomes transparent gradually; For 450ppm hard water, When the suspending agent was added, there was precipitation in the water, which gradually disappeared after continued stirring, and the system gradually became transparent; when adding 200ppm hard water, it was slightly turbid, but the system quickly became transparent; for pure water, except for a small amount of particles when adding No precipitation or turbidity is seen; when the suspending agent formulation is added to water according to the stated dosage, the amount of sodium polyphosphate added can be used to meet the stated amount of 800ppm hard water and can be completely complexed The amount of calcium and magnesium ions in it.

The viscosity of the aqueous suspension obtained in the above examples is between 75-105mpa.s, which can fully meet the requirements of coccidia suspension. For the required viscosity and suspension, it can be adjusted according to the actual situation to meet a wider range of requirements.

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and various changes can also be made to the above embodiments of the present invention. That is to say, all simple and equivalent changes and modifications made according to the claims and description of the application for the present invention fall within the protection scope of the claims of the patent of the present invention. What is not described in detail in the present invention is conventional technical content.

Claims

A kind of suspending agent, it is characterized in that, described suspending agent is used for forming the aqueous medium with water suspending property according to dosage, especially when being used for forming aqueous medium with the water hardness of 180～1000ppm, it has visual characteristics, its The composition includes the following components in weight percentage: 0.1-30% polyacrylate monovalent salt, 0.1-50% visual characteristic reagent, 0.1-50% rheological property regulator, 0.1-90% fluidity property regulator,

The visualization feature reagent is selected from polyphosphate monovalent salts and/or chelating agents containing amino and carboxyl groups,

The visual feature is that after the suspending agent is added to the water, precipitation and/or turbidity occurs first, and then the precipitation and/or the turbidity disappears. The influence of rheological properties has been basically eliminated, and the aqueous medium with the required viscosity has been obtained,

Wherein the dose is 3-50 g of the suspending agent added to 1 L of the water, and the viscosity of the aqueous medium is 20 mpa.s to 500 mpa.s.
The suspending agent according to claim 1, wherein the polyacrylate monovalent salt is selected from one or more mixtures of sodium polyacrylate, potassium polyacrylate, lithium polyacrylate, and ammonium polyacrylate.
The suspending agent according to claim 1 or 2, wherein the polyphosphate monovalent salt is selected from one of sodium polyphosphate, potassium polyphosphate, lithium polyphosphate, and ammonium polyphosphate. a mixture of one or more.
The suspending agent according to claim 1 or 2, wherein the chelating agent containing amino and carboxyl groups is selected from EDTA salts.
The suspending agent according to claim 4, wherein the EDTA salt is selected from disodium EDTA and/or dipotassium EDTA and/or dilithium EDTA and/or diammonium EDTA.
The suspending agent according to claim 1 or 2, wherein the rheology regulator is selected from alkali metal salts and/or ammonium salts.
The suspending agent according to claim 6, wherein the alkali metal salt is selected from hydrochloride, sulfate, sulfite, thiosulfate, hydrobromide, hydroiodic acid of alkali metal ions a mixture of one or more of salts and nitrates, and/or

The ammonium salt is selected from one or more mixtures of ammonium ion hydrochloride, sulfate, sulfite, thiosulfate, hydrobromide, hydroiodide and nitrate.
The suspending agent according to claim 1 or 2, wherein the fluidity regulator is selected from fumed silica, precipitated silica, anhydrous sodium sulfate, anhydrous glucose, spherical silica, A mixture of one or more of talcum powder and mica powder.
A kind of suspending agent, it is characterized in that, described suspending agent has visualization characteristic when being used for forming aqueous medium with the water that hardness is 180～1000ppm according to dose, it comprises the following component of weight percent: polyacrylic acid root- Valence salt 3-25%, visual characteristic reagent 10-40%, rheological performance modifier 1-30%, flow performance modifier 40-80%,

The visualization feature reagent is selected from polyphosphate monovalent salt and/or EDTA salt,

The polyacrylate monovalent salt is selected from one or more mixtures of sodium polyacrylate, potassium polyacrylate, lithium polyacrylate, and ammonium polyacrylate,

The polyphosphate root monovalent salt is selected from one or more mixtures of sodium polyphosphate, potassium polyphosphate, lithium polyphosphate, and ammonium polyphosphate,

The EDTA salt is selected from disodium EDTA and/or dipotassium EDTA,

The rheology modifier is selected from alkali metal salts and/or ammonium salts, and

The fluidity regulator is selected from one or more mixtures of fumed silica, precipitated silica, anhydrous sodium sulfate, anhydrous glucose, and spherical silica;

The visual feature is that after the suspending agent is added to the water, precipitation and/or turbidity occurs first, and then the precipitation and/or the turbidity disappears,

When the visual feature is displayed, it shows that the influence of the hardness of water on the rheological properties of the system has been basically eliminated, and the aqueous medium with the required viscosity for suspending coccidiosis vaccines, medicines or additives has been obtained,

Wherein the dose is 3-20 g of the suspending agent added to 1 L of the water, and the viscosity of the aqueous medium is 20 mpa.s to 500 mpa.s.
The suspending agent according to claim 9, wherein the alkali metal salt is selected from hydrochloride, sulfate, sulfite, thiosulfate, hydrobromide, hydroiodic acid of alkali metal ions a mixture of one or more of salts and nitrates, the alkali metal ions being sodium, potassium or lithium ions, and/or

The ammonium salt is selected from one or more mixtures of ammonium ion hydrochloride, sulfate, sulfite, thiosulfate, hydrobromide, hydroiodide and nitrate.
The suspending agent according to claim 10, characterized in that, the suspending agent is used to form an aqueous medium with water having a hardness of 180-800 ppm.
A suspending agent, characterized in that, the suspending agent is used to form an aqueous medium with water having a hardness of 180-500 ppm, and it consists of the following components in weight percent:

Sodium polyacrylate 5-25%, sodium polyphosphate and/or disodium EDTA 10-25%, sodium chloride and/or potassium chloride and/or ammonium chloride and/or sodium sulfate and/or potassium sulfate and /or ammonium sulfate and/or sodium thiosulfate and/or potassium thiosulfate and/or ammonium thiosulfate 2-25%, fumed silica and/or precipitated silica and/or spherical silica 0.5- 10%, the balance is anhydrous glucose,

Wherein, the sodium polyphosphate and/or disodium EDTA are visualization characteristic reagents, and the visualization characteristic is that after adding the suspending agent in the hard water, precipitation and/or turbidity occur first, and then the precipitation and/or said cloudiness disappears,

When the visual feature is displayed, it indicates that the influence of water hardness on the rheological properties of the system has been basically eliminated, and the water medium with the required viscosity has been obtained.

Wherein the dose is 3-20g of the suspending agent added to 1L of the water, and the viscosity of the aqueous medium is 20mpa.s-500mpa.s.
Use of the suspending agent according to any one of claims 1-12 in the preparation of an aqueous suspension of a coccidial vaccine, medicine or additive.
The use according to claim 13, characterized in that the coccidia vaccine is preferably selected from coccidia oocyst vaccines.
purposes according to claim 14, is characterized in that, described coccidiosis oocyst vaccine is selected from chicken coccidia oocyst vaccine, rabbit coccidia oocyst vaccine, pigeon coccidia oocyst vaccine, duck coccidia oocyst vaccine, Pig coccidia oocyst vaccine, bovine coccidia oocyst vaccine, canine coccidia oocyst vaccine.
The preparation method of the suspending agent described in any one of claims 1-12, is characterized in that, described preparation method comprises first part or all of described fluidity conditioner and polyacrylate radical monovalent salt mixing, then add The visualization feature reagent, the rheology regulator and the rest of the fluidity regulator may be uniformly mixed.