Method for preventing caking of lysine feed additive

WO2026168915A1PCT designated stage Publication Date: 2026-08-13CJ CHEILJEDANG CORP
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Patent Information

Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Filing Date
2026-02-03
Publication Date
2026-08-13
Patent Text Reader

Abstract

The present disclosure relates to a method for preventing caking of a lysine feed additive and, specifically, to a composition for preventing caking of a lysine feed additive, and a method for preventing caking of a lysine feed additive by using same, the composition being capable of suppressing the occurrence of caking of a lysine feed additive and improving long-term storage stability.
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Description

Method to prevent solidification of lysine feed additives

[0001] The present disclosure relates to a method for preventing solidification of a lysine feed additive, and specifically to a composition for preventing solidification of a lysine feed additive capable of suppressing solidification of the lysine feed additive and improving long-term storage stability, and a method for preventing solidification of a lysine feed additive using the same.

[0002]

[0003] A potential issue during the storage and transportation of manufactured products is caking. Caking is influenced by extrinsic factors such as moisture, temperature, pressure / stress, mixing, electric fields, and time, as well as intrinsic factors of the powder particles, including chemical composition, molecular weight, surface charge / polarity, physical state, size, and shape (linear / plate-like / spherical). These factors affect various reactions (hydration, solubilization, deliquescence, decomposition, etc.), phase transitions (glass-rubber transition, recrystallization, solidification, etc.), and particle redistribution (attrition, segregation, etc.) during processes such as heating or cooling, moisture absorption or drying, pressurization, and handling. Consequently, the viscosity of the particle surface increases, and liquid / solid bridges are formed, leading to solidification through sintering and interlocking. Liquid / solid bridges between powder particles are formed by various causes, such as the influx of moisture and drying, the melting and solidification of lipids, the dissolution and drying of solutes, and crystallization (Effects of anticaking agents and storage conditions on the moisture sorption, caking, and flowability of deliquescent ingredients, Food Research International, Volume 45, Issue 1, January 2012, Pages 369-380). Caking is a difficult problem that occurs due to the various causes mentioned above and requires industrial resolution.

[0004] On the other hand, lysine carries a positive charge in the absence of a counterpart ion and is highly reactive with moisture. This leads to increased hygroscopicity and solidification. To prevent this, counterpart ions are provided for lysine, such as hydrochloric acid, sulfuric acid, or carbonic acid. However, even if hygroscopicity is reduced by providing such counterpart ions, particle clumping occurs during long-term storage or transport, resulting in solidification.

[0005] Therefore, for feed additives containing lysine, a manufacturing method capable of improving storage stability by suppressing solidification is required.

[0006]

[0007] The present disclosure aims to provide a composition for preventing solidification of a lysine feed additive and a method for preventing solidification of a lysine feed additive using the same, which can suppress the occurrence of solidification of the lysine feed additive and improve long-term storage stability.

[0008]

[0009] One objective of the present disclosure is to provide a lysine feed additive composition for preventing solidification, comprising calcium stearate.

[0010] Another objective of the present disclosure is to provide a method for preventing solidification of a lysine feed additive using the composition for preventing solidification of a lysine feed additive of the present disclosure.

[0011]

[0012] The anti-solidification composition and anti-solidification method of the present disclosure can provide a lysine feed additive with a high lysine content with a minimum amount of anti-solidification agent, as well as improved storage safety by suppressing the occurrence of solidification through the addition of an anti-solidification agent to a lysine feed additive with high hygroscopicity.

[0013]

[0014] This is explained in detail as follows. Meanwhile, each description and embodiment disclosed in this disclosure may also be applied to other descriptions and embodiments. That is, all combinations of the various elements disclosed in this disclosure fall within the scope of this disclosure. Furthermore, the scope of this disclosure should not be considered limited by the specific descriptions provided below.

[0015]

[0016] To achieve the above objective, one aspect of the present disclosure provides a composition for preventing lysine carbonate solidification comprising calcium stearate.

[0017]

[0018] The anti-solidification composition of the present disclosure may include calcium stearate in a lysine feed additive to solve the problem of solidification of lysine products occurring in the feed additive industry, and the anti-solidification method of the present disclosure may suppress solidification by adding calcium stearate in powder form and mixing.

[0019] The term "calcium stearate" in this disclosure refers to a carboxylate salt of calcium, and its chemical formula, which may be added to food, is C 36 H 70 It refers to a compound of CaO4. When the above calcium stearate is added to a lysine feed additive, it can suppress the solidification of lysine, which has very high reactivity with moisture, thereby improving clumping and storage safety.

[0020]

[0021] The above lysine feed additive refers to a feed additive containing lysine, and generally, it may be provided in the form of a salt by providing a counterpart ion of lysine. Specifically, the above lysine feed additive may be lysine hydrochloride, lysine sulfate, or lysine carbonate, and specifically, it may be lysine carbonate; in this case, the counterpart ion of lysine is provided to reduce reactivity with moisture, thereby reducing hygroscopicity. Additionally, it may be in the form of a powder or granules to be suitable for use as a feed additive.

[0022] The lysine content in the above lysine carbonate may be included in an amount of 70 to 85 weight%, and specifically in an amount of 76 to 80 weight%.

[0023] The above lysine carbonate can be prepared by fermenting a lysine-producing strain, such as a lysine-producing Corynebacterium glutamicum strain, to obtain an L-lysine fermentation liquid, and then injecting carbon dioxide into the fermentation liquid, and accordingly, carbonate or bicarbonate may be included. The content of the carbonate or bicarbonate may be 2 to 23 weight%, specifically 2 to 19 weight%, 3 to 22 weight%, 3 to 18 weight%, or 6 to 15 weight%.

[0024] The pH of the above lysine carbonate may be 8 to 10, specifically 8.5 to 9.5.

[0025]

[0026] Another aspect of the present disclosure provides a method for preventing solidification of lysine carbonate granules, comprising the step of adding calcium stearate to lysine carbonate granules.

[0027] Here, calcium stearate and solidification prevention are as described above.

[0028] The above calcium stearate may be introduced in powder form.

[0029] Among the various formulations and types of commercially available lysine feed additives, the calcium stearate of the present disclosure has excellent effects in preventing solidification and inhibiting solidification, particularly with respect to lysine carbonate granules.

[0030] The above calcium stearate can exhibit excellent solidification prevention and solidification inhibition effects with only a small amount added relative to lysine carbonate granules. Specifically, when added in powder form, it can be added at 0.1 to 0.5% (w / w) relative to lysine carbonate granules, and more specifically, it can be added at 0.2 to 0.5% (w / w), 0.25 to 0.5% (w / w), 0.1 to 0.4% (w / w), 0.1 to 0.3% (w / w), 0.2 to 0.4% (w / w), 0.2 to 0.3% (w / w), 0.2 to 0.25% (w / w), 0.25 to 0.3% (w / w), or 0.25% (w / w).

[0031] In addition, the calcium stearate may be added in an amount of 0.1 to 0.7% (w / w) relative to lysine in the lysine carbonate, and specifically, may be added in an amount of 0.1 to 0.6% (w / w), 0.2 to 0.5% (w / w), 0.3 to 0.4% (w / w), or 0.3 to 0.35% (w / w).

[0032] In addition, the calcium stearate may be added in an amount of 0.5 to 10% (w / w) relative to the carbonate or bicarbonate in the lysine carbonate, and specifically, may be added in an amount of 0.6 to 8.5% (w / w) or 1 to 5% (w / w).

[0033] In this case, an excellent solidification inhibition effect is achieved even with a small amount of anti-solidification agent, which reduces costs and allows for the maintenance of a high lysine content in lysine feed additives, specifically lysine carbonate.

[0034]

[0035] The above anti-solidification method may be a combination of a lower limit selected from 55%, 60%, 64%, 70%, 80%, or 85%, and an upper limit selected from 100%, 95%, 90%, 86%, or 85%, with a lump reduction rate of 50% or more.

[0036] In the present disclosure, the term "lumping" refers to confirming the amount of lumps that have solidified and clumped together in the powder, and "lumping reduction rate" refers to the degree to which the amount of lumps is reduced compared to the absence of an anti-solidification agent.

[0037] The measurement of the above lumps may involve separating solidified lumps from the powder and measuring their mass, or storing the powder under accelerated solidification conditions to measure the lumps. For example, the powder with an anti-solidification agent added may be stored in a constant temperature and humidity chamber (30°C, RH 60%) for 24 hours, then compressed (7 bar, 10 minutes) to accelerate solidification, and then the solidified lumps may be separated through a mesh screen and their mass measured.

[0038]

[0039] After performing the above anti-solidification method, the lump breakage rate may be 90% or more, specifically 95% or more, 98% or more, or 99% or more.

[0040] In the present disclosure, the term "lump breakage rate" refers to the release of a solidified lump from its solidified state due to an external stimulus, and the external stimulus may include vibration, crushing, sieving, etc.

[0041] The measurement of the above-mentioned lump breakage rate involves separating solidified lumps from the powder and measuring the breakage of the lumps by applying an external stimulus, and conventional methods can be used without limitation. For example, the solidified lumps of the sample may be separated through a mesh, and the degree of breakage may be measured by applying vibration to the solidified lumps.

[0042]

[0043] The present disclosure is described in more detail below by way of examples. However, the following examples are merely preferred embodiments for illustrating the present disclosure and are therefore not intended to limit the scope of the rights of the present disclosure. Meanwhile, technical matters not described in this specification can be sufficiently understood and easily implemented by a person skilled in the art who is proficient in the technical field of the present disclosure or a similar technical field.

[0044]

[0045] Example: Evaluation of Solidification Occurrence of Lysine Feed Additive According to Addition of Anti-solidification Powder

[0046]

[0047] To optimize the anti-caking agent and content suitable for lysine feed additives, an evaluation of solidification occurrence was conducted when anti-caking agent powder was added and mixed for each of the commercially produced lysine sulfate granules (CJ CheilJedang, Korea) and lysine carbonate granules produced based on a disclosed method (Korean Patent Publication KR10-2020-0073298A and US Patent Publication US2022-0030914A1).

[0048] Specifically, lysine carbonate granules were prepared by fermenting a lysine-producing Corynebacterium glutamicum strain to obtain an L-lysine fermentation liquid, and then obtaining an L-lysine aqueous solution through cell removal, etc. Carbon dioxide was injected into the L-lysine aqueous solution to contain carbonate ions, and lysine carbonate granules were prepared through spray granulation.

[0049] The above lysine carbonate granules contained 76-80 wt% lysine, 6-15 wt% bicarbonate, and a pH of 8.5-9.5.

[0050] To optimize the suitable anti-caking agent and content for lysine feed additives, an evaluation of solidification occurrence was conducted when anti-caking agent powder was added and mixed into commercially produced lysine feed additives.

[0051] First, in this embodiment, two types of lysine feed additives were used: lysine sulfate granules (CJ CheilJedang, Korea) and lysine carbonate granules (CJ CheilJedang, Korea).

[0052]

[0053] Example 1: Confirmation of the effect of inhibiting solidification according to the type of lysine feed additive

[0054]

[0055] First, calcium stearate (JUNSEI CHEMICAL) was used as an anti-solidification agent, and the effect of inhibiting solidification was evaluated when the anti-solidification agent was added / mixed according to each lysine feed additive.

[0056] Specifically, 140 g of lysine carbonate granules or lysine sulfate granules were placed in a 500 ml PE bottle, and 0.25% and 0.5% (w / w) of calcium stearate powder were added to the product weight, respectively, and the bottles were sealed. Then, the PE bottles containing the lysine feed additive product and the anti-caking agent were connected to a stirrer (Daihan scientific, HT-50AX) and mixed at 40 rpm for 10 minutes.

[0057] Subsequently, to evaluate the occurrence of solidification in lysine carbonate granules and lysine sulfate granules with and without the addition of anti-solidification powder, 140 g each of the product mixed with the anti-solidification powder and the product without the powder were placed in a constant temperature and humidity chamber (TH3-E-200, JeioTech Co.) under conditions of 30 °C and RH 60%. After 24 hours, the products, having completed moisture absorption, were placed in a PE bag (14 cm X 14 cm) and compressed for 10 minutes at a pressure of 7 bar. The compressed samples were placed on a mesh screen (12 mesh, Daihan scientific), the PE bag was removed, and the clumping rate was measured. The reduction rate of clumping when the anti-solidification powder was added was calculated based on the clumping rate when the anti-solidification powder was not added. Afterwards, the mesh containing the product was transferred to a vibrating device (Minoe 200, Endecotts) and subjected to vibration at 50 Hz for 5 minutes to measure the rate of breakage of the resulting lumps.

[0058]

[0059] Product Lysine Carbonate Granules Lysine Sulfate Granules Item Calcium Stearate Calcium Stearate Anti-caking Agent Addition Method Powder Mix Powder Mix Anti-caking Agent Addition Amount (wt%) 0.0 0.2 5 0.5 0.0 0.2 5 0.5 Clump Reduction Rate (%) -6 4 8 6 -4 5 8 6 Clump Breakage Rate (%) 10 0.0 10 0.0 10 0.0 5 2.7 6 9.5 8 6.7

[0060]

[0061] As a result, as shown in Table 1 above, it was confirmed that clumping was significantly reduced in lysine carbonate granules with only a small amount (about 0.25 wt%) of calcium stearate added compared to lysine sulfate granules. In addition, it was confirmed that the clumping rate of lysine carbonate granules was 100%. Through this, it was confirmed that when calcium stearate is powdered and added as an anti-caking agent to lysine carbonate granules, an excellent effect of inhibiting solidification can be achieved while maintaining a high content of lysine within the lysine feed additive, with only a small amount of anti-caking agent added.

[0062]

[0063] Example 2: Confirmation of solidification inhibition effect according to the type of anti-solidification agent

[0064]

[0065] Through Example 1-1 above, it was confirmed that calcium stearate has an excellent effect in inhibiting solidification on lysine carbonate granules as an anti-solidification agent, and thus it was intended to be compared with other anti-solidification agents.

[0066] In addition to calcium stearate, silicon dioxide (DAEJUNG), milled silicon dioxide (DAEJUNG), and calcium phosphate (DAEJUNG) were used as anti-caking agents.

[0067] The method for adding anti-caking agent and measuring the lump aggregation reduction rate / lump breakage rate is the same as in Example 1.

[0068]

[0069] Product Lysine Carbonate Granules Item Calcium stearate Calcium phosphate Silicon dioxide Milled silicon dioxide Anti-caking Agent Addition Method Powder Mixed Powder Mixed Powder Mixed Powder Mixed Anti-caking Agent Addition Amount (wt%) 0.0 0.2 5 0.5 0.00.2 5 0.5 0.00.2 5 0.5 0.00.2 5 0.5 Clumping Rate (%) 16.0 5.8 2.3 16 7.2 3.7 16 11.5 7.8 16 9.1 5.6 Clumping Reduction Rate (%) -6 48 6 -5 57 7 -2 85 1 -4 36 5 Clumping Breakage Rate (%) 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0

[0070]

[0071] As a result, as shown in Table 2 above, it was confirmed that when calcium stearate was used as an anti-solidification agent, the reduction rate of lump formation was significantly superior compared to other anti-solidification agents. Meanwhile, the lump breakage rate was excellent for all anti-solidification agents. Through this, it was confirmed that when calcium stearate is powdered and added to lysine carbonate granules as an anti-solidification agent, it can exhibit a superior effect in inhibiting solidification compared to other anti-solidification agents.

[0072]

[0073] As a result, it was confirmed that the combination of lysine carbonate granules as a lysine feed additive and calcium stearate as an anti-solidification agent is an excellent combination for inhibiting solidification.

[0074]

[0075] From the foregoing description, those skilled in the art to which this disclosure pertains will understand that this disclosure may be implemented in other specific forms without altering its technical concept or essential features. In this regard, the embodiments described above should be understood as illustrative in all respects and not restrictive. The scope of this disclosure should be interpreted as including all modifications or variations derived from the meaning and scope of the claims set forth below and their equivalents, rather than from the detailed description above.

Claims

1. A method for preventing solidification of lysine carbonate granules, comprising the step of adding calcium stearate to lysine carbonate granules.

2. In Paragraph 1, A method for preventing solidification of lysine carbonate granules, wherein the above calcium stearate is introduced in powder form.

3. In Paragraph 1, A method for preventing solidification of lysine carbonate granules, wherein the calcium stearate is added at 0.1 to 0.5% (w / w) relative to the lysine carbonate granules.

4. In Paragraph 1, The above method for preventing solidification is a method for preventing solidification of lysine carbonate granules, wherein the reduction rate of lump formation is 50% or more compared to lysine carbonate granules without calcium stearate.

5. In Paragraph 1, The above method for preventing solidification is a method for preventing solidification of lysine carbonate granules having a lump aggregation breakage rate of 90% or more.