A fatty acid diethylaminoethanol ester citrate

Abstract

This invention belongs to the field of plant growth regulator technology, and particularly relates to a fatty acid diethylaminoethanol ester citrate. The fatty acid diethylaminoethanol ester citrate provided by this invention is composed of fatty acid diethylaminoethanol ester citrate technical and 4-5% anti-caking agent, wherein the anti-caking agent is composed of silica powder and potassium pyrophosphate. Through the combination of silica powder and potassium pyrophosphate, while potassium pyrophosphate fixes the surface moisture of the fatty acid diethylaminoethanol ester citrate technical, the silica powder encapsulates and blocks the capillaries on the surface of the technical, preventing the migration of moisture inside the technical particles. This synergistically improves the anti-caking performance of the fatty acid diethylaminoethanol ester citrate technical under high temperature and high humidity conditions, enabling the technical to maintain a high anti-caking rate under conditions below 50°C and humidity not exceeding 90%.

Description

Technical Field

[0001] This invention belongs to the field of plant growth regulator technology, and particularly relates to a fatty acid diethylaminoethanol ester citrate. Background Technology

[0002] Diethylaminoethanol fatty acid citrate (DA-X citrate), as a plant growth regulator, is widely applicable to various soils and crops. It can increase the content of chlorophyll, protein, and nucleic acid in plants and improve photosynthesis; enhance the activity of peroxidase and nitrate reductase; promote carbon and nitrogen metabolism in plants; enhance the absorption of water and fertilizer and the accumulation of dry matter; regulate the water balance in plants; and enhance the disease resistance, drought resistance, and drought tolerance of crops and fruits and vegetables. At the same time, it can delay plant acid senescence, promote early maturity, increase yield, and improve crop quality.

[0003] DA-X citrate technical material is in powder form at room temperature. However, DA-X citrate technical material is very hygroscopic and is prone to dehydration and recrystallization at high temperatures, which causes it to clump together and make the technical material clumpy. This makes DA-X citrate technical material inconvenient in production, storage, transportation and use. Summary of the Invention

[0004] The purpose of this invention is to provide a fatty acid diethylaminoethanol ester citrate, which solves the problem that the technical grade fatty acid diethylaminoethanol ester citrate is prone to caking under high temperature and high humidity conditions, causing inconvenience in production, storage, transportation and use.

[0005] To solve the above-mentioned technical problems, the technical solution of the present invention for fatty acid diethylaminoethanol ester citrate is as follows:

[0006] A fatty acid diethylaminoethanol ester citrate, comprising fatty acid diethylaminoethanol ester citrate technical and 4-5% anti-caking agent, wherein the anti-caking agent is composed of silica powder and potassium pyrophosphate.

[0007] This invention improves upon existing technology by providing fatty acid diethylaminoethanol ester citrate. An anti-caking agent is added to the technical grade of fatty acid diethylaminoethanol ester citrate. This is achieved through a combination of silica powder and potassium pyrophosphate. While potassium pyrophosphate fixes the surface moisture of the technical grade, silica powder encapsulates and blocks the capillaries on the surface of the technical grade, preventing moisture migration from within the particles. This synergistically improves the anti-caking performance of the technical grade under high temperature and high humidity conditions, enabling it to maintain a high anti-caking rate under conditions below 50°C and humidity not exceeding 90%.

[0008] To further improve the anti-caking ability of fatty acid diethylaminoethanol ester citrate under high temperature and high humidity conditions, preferably, the mass ratio of silica powder to potassium pyrophosphate is 3:(1-3).

[0009] To further improve the anti-caking properties of diethylaminoethanol citrate fatty acid under high humidity conditions, preferably, the mass ratio of silica powder to potassium pyrophosphate is 3:(1-2).

[0010] To further improve the anti-caking properties of diethylaminoethanol citrate of fatty acid and reduce the agglomeration rate to less than 35%, it is preferably composed of diethylaminoethanol citrate of fatty acid technical and 5% anti-caking agent, wherein the mass ratio of silica powder to potassium pyrophosphate is 3:2.

[0011] To further improve the anti-caking properties of fatty acid diethylaminoethanol ester citrate under high-temperature conditions, preferably, the fatty acid diethylaminoethanol ester citrate technical material includes diethylaminoethanol hexanoate citrate technical material, diethylaminoethanol octanoate citrate technical material, and diethylaminoethanol decanoate citrate technical material. The alkyl groups of fatty acid diethylaminoethanol ester citrate are sensitive to temperature changes, which affect the state of the technical material and thus its anti-caking properties.

[0012] To further prevent moisture migration within the drug particles, preferably, the silica powder is prepared by vapor deposition.

[0013] To further improve the clogging efficiency of the capillary pores on the surface of the active ingredient, preferably, the particle size of the silica powder is 12nm to 19μm.

[0014] In order to further reduce the agglomeration rate by improving the clogging efficiency of the capillary pores on the surface of the active ingredient, and to make the agglomeration rate less than 45%, preferably, the particle size of the silica powder is 12-15 nm. Attached Figure Description

[0015] Figure 1 A bar graph showing the agglomeration rate of DA-X citrate technical grade at different temperatures;

[0016] Figure 2 Graph showing the morphological changes of DA-X citrate technical grade at different temperatures;

[0017] Figure 3 A bar graph showing the water content of DA-X citrate technical grade at different temperatures;

[0018] Figure 4 A bar graph showing the agglomeration rate of DA-X citrate technical grade under different humidity conditions;

[0019] Figure 5The graph shows the morphological changes of DA-X citrate technical grade under different humidity conditions;

[0020] Figure 6 A bar chart showing the water content of DA-X citrate technical grade under different humidity levels;

[0021] Figure 7 Bar graphs showing the agglomeration rate of DA-X citrate technical grade with a single anti-caking agent introduced at different temperatures;

[0022] Figure 8 Graph showing the morphological changes of DA-X citrate technical grade drug after introducing a single anti-caking agent at different temperatures;

[0023] Figure 9 A bar graph showing the water content of DA-X citrate technical grade with a single anti-caking agent introduced at different temperatures;

[0024] Figure 10 A bar graph showing the agglomeration rate of DA-X citrate technical grade under high humidity conditions with the introduction of a single anti-caking agent;

[0025] Figure 11 A graph showing the morphological changes of DA-X citrate technical grade under high humidity conditions after the introduction of a single anti-caking agent.

[0026] Figure 12 A bar graph showing the water content of DA-X citrate technical grade under high humidity conditions, with the introduction of a single anti-caking agent. Detailed Implementation

[0027] The technical concept of fatty acid diethylaminoethanol ester citrate provided by this invention is as follows:

[0028] A fatty acid diethylaminoethanol ester citrate, comprising fatty acid diethylaminoethanol ester citrate technical and 4-5% anti-caking agent, said anti-caking agent comprising silica powder and potassium pyrophosphate. Diethylaminoethanol ester citrate (DA-X citrate) technical grade is prone to clumping due to the temperature sensitivity of its alkyl fatty alcohol chains, which cause state transitions during temperature changes. Furthermore, its water solubility allows it to absorb moisture in high humidity environments, leading to dissolution of the particle surface and the formation of "crystal bridges" between closely spaced particles, further contributing to clumping. This invention addresses this by combining silica powder and potassium pyrophosphate. While potassium pyrophosphate fixes the surface moisture of DA-X citrate technical grade, silica powder encapsulates and blocks the capillaries on the surface, preventing internal moisture migration. This synergistic effect improves the anti-caking properties of DA-X citrate technical grade under high temperature and high humidity conditions, enabling it to maintain a high anti-caking rate at temperatures below 50°C and humidity levels not exceeding 90%.

[0029] In a specific embodiment, the fatty acid diethylaminoethanol ester citrate (DA-X citrate) technical material includes diethylaminoethanol hexanoate citrate (DA-6 citrate) technical material, diethylaminoethanol caprylate citrate (DA-8 citrate) technical material, and diethylaminoethanol capricate citrate (DA-10 citrate) technical material, wherein the chemical formula of DA-6 citrate technical material is C 18 H 33 NO9, its chemical structure is shown in Formula I:

[0030]

[0031] The chemical formula of DA-8 citrate technical is C 20 H 37 NO9, chemical structure as shown in Formula II:

[0032]

[0033] The chemical formula of DA-10 citrate technical grade is C 22 H 41 NO9, its chemical structure is shown in Formula III:

[0034]

[0035] DA-6, DA-8 and DA-10 citrate technical materials have similar biological activities and are all in powder form at room temperature.

[0036] In a specific embodiment, the silica powder is produced by Evonik Industries, Inc. 22LS, produced by Kaiyin Chemical Co., Ltd. 820A, the The powder particle size of 22LS is 12-19 μm. The powder particles of 820A have a particle size of 12-15 nm and are all prepared by vapor deposition.

[0037] In a specific embodiment, the preparation method of the fatty acid diethylaminoethanol ester citrate includes the following steps: adding the appropriate mass of silica powder and potassium pyrophosphate to the fatty acid diethylaminoethanol ester citrate technical material and mixing evenly to obtain the product.

[0038] The embodiments of the present invention will be further described below with reference to specific examples. Unless otherwise specified, the chemical reagents involved in the following examples are all commercially available conventional products. The DA-6, DA-8, and DA-10 citrate technical materials were purchased from Zhengzhou Zhengshi Chemical Products Co., Ltd., with a content of 98% and a particle size greater than 60 mesh; the potassium pyrophosphate was purchased from Shifang Zhixin Chemical Co., Ltd.; the anti-caking agent 1 was purchased from Zibo Yuhang Co., Ltd., with anhydrous magnesium sulfate as the active ingredient; the anti-caking agent 2 was purchased from Tianjin Longhua Co., Ltd.; the nano-alumina and NT-104 were purchased from Guangzhou Huiyong Polymer Materials Co., Ltd.; and the Petro AG was purchased from Akzo Inc.

[0039] I. Specific Examples of Fatty Acid Diethylaminoethanol Ester Citrate of the Present Invention

[0040] The fatty acid diethylaminoethanol ester citrate of the present invention has the following formulation as shown in Table 1.

[0041] Table 1. Formulation composition of fatty acid diethylaminoethanol ester citrate

[0042]

[0043]

[0044] Example 1, a fatty acid diethylaminoethanol ester citrate, comprises 96% DA-6 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 3%. 22LS, 1% potassium pyrophosphate;

[0045] Example 2's fatty acid diethylaminoethanol ester citrate comprises 95% DA-6 citrate technical grade and 5% anti-caking agent, wherein the anti-caking agent is 3%. 22LS, 2% potassium pyrophosphate;

[0046] Example 3, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-6 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 2%. 22LS, 2% potassium pyrophosphate;

[0047] Example 4's fatty acid diethylaminoethanol ester citrate comprises 96% DA-6 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 3%. 820A, 1% potassium pyrophosphate;

[0048] Example 5, fatty acid diethylaminoethanol ester citrate, comprises 95% DA-6 citrate technical grade and 5% anti-caking agent, wherein the anti-caking agent is 3%. 820A, 2% potassium pyrophosphate;

[0049] Example 6, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-6 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 2%. 820A, 2% potassium pyrophosphate;

[0050] Example 7's fatty acid diethylaminoethanol ester citrate comprises 96% DA-8 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 3%. 22LS, 1% potassium pyrophosphate;

[0051] Example 8, a fatty acid diethylaminoethanol ester citrate, comprises 95% DA-8 citrate technical grade and 5% anti-caking agent, wherein the anti-caking agent is 3%. 22LS, 2% potassium pyrophosphate;

[0052] Example 9, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-8 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 2%. 22LS, 2% potassium pyrophosphate;

[0053] Example 10, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-8 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 3%. 820A, 1% potassium pyrophosphate;

[0054] Example 11, fatty acid diethylaminoethanol ester citrate, comprises 95% DA-8 citrate technical grade and 5% anti-caking agent, wherein the anti-caking agent is 3%. 820A, 2% potassium pyrophosphate;

[0055] Example 12, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-8 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 2%. 820A, 2% potassium pyrophosphate;

[0056] Example 13, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-10 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 3%. 22LS, 1% potassium pyrophosphate;

[0057] Example 14, fatty acid diethylaminoethanol ester citrate, comprises 95% DA-10 citrate technical grade and 5% anti-caking agent, wherein the anti-caking agent is 3%. 22LS, 2% potassium pyrophosphate;

[0058] Example 15, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-10 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 2%. 22LS, 2% potassium pyrophosphate;

[0059] Example 16, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-10 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 3%. 820A, 1% potassium pyrophosphate;

[0060] Example 17, fatty acid diethylaminoethanol ester citrate, comprises 95% DA-10 citrate technical grade and 5% anti-caking agent, wherein the anti-caking agent is 3%. 820A, 2% potassium pyrophosphate;

[0061] Example 18, fatty acid diethylaminoethanol ester citrate, comprises 96% DA-10 citrate technical grade and 4% anti-caking agent, wherein the anti-caking agent is 2%. 820A, 2% potassium pyrophosphate.

[0062] II. Experimental Examples

[0063] In the following experimental examples, the agglomeration properties of samples under different temperatures and humidity levels were tested according to the following methods:

[0064] 1. Agglomeration performance test at different temperatures

[0065] (1) Take fatty acid diethylaminoethanol ester citrate with different formulations as test samples, 4 portions of each test sample, 20 grams of each portion;

[0066] (2) Place the four test samples into 50ml square transparent PE bottles respectively, and seal the bottle openings with a sealing machine to prevent gas from entering;

[0067] (3) Place the sealed PE bottle into a constant temperature oven at different temperatures: 25℃, 35℃, 45℃ and 50℃. Close the oven door and maintain the internal temperature of the oven.

[0068] (4) After placing the sample in a constant temperature oven for 2 days, remove the sample from the oven.

[0069] 2. Agglomeration performance test under different humidity levels

[0070] (1) Take fatty acid diethylaminoethanol ester citrate with different formulations as test samples, one sample of each type, 20 grams;

[0071] (2) Place the test samples into 50ml square transparent PE bottles and leave the bottle openings open;

[0072] (3) Place the PE bottle into a humidity control box with different humidity levels. Set the temperature of the humidity control box to 25°C and the humidity to 90%. Close the door of the humidity control box and maintain the temperature and humidity inside the control box.

[0073] (4) After placing the sample in the humidity control box for 2 days, remove the test sample from the control box.

[0074] 3. Calculation method for sample agglomeration rate

[0075] Cut open the PE bottles that have been placed at different temperatures for 2 days from the top, without cutting into the sample; then pour out the test samples from the PE bottles that have been placed at different temperatures and humidity levels for 2 days and pass them through a 20-mesh sieve. Powder larger than 20 mesh is considered qualified, and samples smaller than 20 mesh are considered agglomerated. The agglomeration rate is calculated as shown in Formula 1:

[0076]

[0077] 4. Moisture content test of DA-X citrate technical grade

[0078] The moisture content of DA-X citrate technical material after being stored under different temperatures and humidity conditions for a period of time was determined using the loss on drying method. Specifically, the original weight M0 of the DA-X citrate technical material sample was measured to be 4g ± 0.1g. After drying at a constant temperature of 105℃, the weight was measured as M. x The ratio of weight loss before and after constant temperature drying to the original weight is the moisture content.

[0079] This experimental example illustrates the formulation screening results of Examples 1-18.

[0080] 1. Anti-caking performance test of fatty acid diethylaminoethanol ester citrate technical grade

[0081] (1) Agglomeration performance test at different temperatures

[0082] The high-temperature agglomeration rate of DA-6, DA-8, and DA-10 citrate technical materials was tested by placing them at 25℃, 35℃, 45℃, and 50℃ for a period of time. The test results are as follows: Figure 1 As shown, the morphological changes of the original drug are as follows: Figure 2 As shown; and the moisture content of the original drug was tested after being placed at different temperatures for a period of time, and the test results are as follows. Figure 3 As shown.

[0083] from Figure 1-2It can be seen that no clumping occurred in DA-X citrate technical material after 3 days of storage at 25℃. However, with increasing temperature, specifically between 35-45℃, the clumping rate of DA-X citrate technical material significantly increased over time. Specifically, DA-8 and DA-10 citrate technical materials reached 100% clumping rate after 2 days. With further increases in temperature, when the temperature reached above 50℃, all three types of DA-X citrate technical materials clumped within one day. This indicates that temperature is a crucial factor affecting the clumping of DA-X citrate technical material; the higher the temperature, the more severe the clumping phenomenon.

[0084] from Figure 3 It can be seen that the moisture content of the three DA-X citrate technical materials did not change significantly with increasing temperature and longer storage time, indicating that temperature does not affect the clumping properties of DA-X citrate technical materials, but is not affected by the moisture content of the technical materials. The moisture content of DA-6 citrate technical materials is approximately 0.35%, DA-8 citrate technical materials are approximately 0.44%, and DA-10 citrate technical materials are approximately 0.46%. The difference in moisture content among the three DA-X citrate technical materials is caused by the difference in their initial moisture content.

[0085] (2) Agglomeration performance test under different humidity conditions

[0086] The technical grade DA-6, DA-8, and DA-10 citrates were placed at 25°C under ambient humidity conditions of 50%, 60%, 70%, 80%, 85%, and 90% for a period of time to test their high-humidity agglomeration rate. The test results are as follows: Figure 4 As shown, the morphological changes of the original drug are as follows: Figure 5 As shown; and the moisture content of the original drug was tested after being placed in different humidity levels for a period of time, and the test results are as follows. Figure 6 As shown.

[0087] from Figure 4-5 It can be seen that ambient humidity has a significant impact on the caking properties of DA-X citrate technical grade. When the ambient humidity is between 50% and 85%, the higher the humidity, the higher the caking rate of DA-X citrate technical grade; that is, the higher the ambient humidity, the easier it is for the technical grade to caking. Under the same humidity conditions, the caking rate of DA-6 citrate technical grade is slightly lower than that of DA-8 and DA-10 citrate. Figure 5 It can be seen that DA-X citrate technical material with a low agglomeration rate is in powder form. As the ambient humidity increases, the free powder of some agglomerated DA-X citrate technical material becomes smaller. When the agglomeration rate reaches more than 90%, DA-X citrate technical material is in a blocky state with very little or no free powder.

[0088] from Figure 6It can be seen that as the ambient humidity increases, the water content of DA-X citrate technical material increases accordingly, indicating that DA-X citrate technical material is hygroscopic. The higher the ambient humidity, the higher the internal humidity of DA-X citrate technical material. In addition, the hygroscopicity of the three types of DA-X citrate technical materials is not significantly different.

[0089] 2. Anti-caking performance test of fatty acid diethylaminoethanol ester citrate technical grade after introduction of a single anti-caking agent

[0090] (1) Agglomeration performance test at different temperatures

[0091] Add 5% anti-caking agent 1, 1% potassium pyrophosphate, 1% nano-alumina, 1% NT-104, 1% AG, 5% anti-caking agent 2, and 1%, 2%, and 3% of [other ingredients] to the technical grade DA-6, DA-8, and DA-10 citrate, respectively. 22LS; 1%, 2%, 3% 820A was tested, and the agglomeration rate of DA-X citrate with a single anti-caking agent was measured at different temperatures. The test results are shown in Table 2-4, and a bar chart is plotted as follows. Figure 7 As shown, Figure 7 The 5% anti-caking agent in the formula is 5% anti-caking agent 1, and the 5% anti-caking agent is 5% anti-caking agent 2. The changes in the morphology of the original drug at different temperatures are as follows: Figure 8 As shown.

[0092] Table 2. Agglomeration rate of DA-6 citrate with a single anti-caking agent at different temperatures.

[0093]

[0094] Table 3. Agglomeration rate of DA-8 citrate with a single anti-caking agent at different temperatures.

[0095]

[0096]

[0097] Table 4. Agglomeration rate of DA-10 citrate with a single anti-caking agent at different temperatures.

[0098]

[0099] From Table 2-4 and Figure 7-8 It can be seen that, compared with the absence of an anti-caking agent, the introduction of a single anti-caking agent reduced the caking rate of DA-X citrate technical grade from 100% to 0%, with an anti-caking effect of 3%. 820A = 2% 820A = 1% 820A = 5% anti-caking agent 2 > 3% 22LS > 2% 22LS > 1% 22LS > 1% NT-104 > 1% AG > 1% Nano-aluminum chloride > 5% Anti-caking agent 1 (anhydrous magnesium sulfate) > 1% potassium pyrophosphate > No anti-caking agent added. Anhydrous magnesium sulfate and potassium pyrophosphate achieve their anti-caking effect by fixing the surface moisture of DA-X citrate technical material; nano-alumina, NT-104, AG anti-caking agent, 22LS and 820A works by encapsulating and blocking the capillaries on the surface of the original drug, thus preventing clumping.

[0100] The dosage includes 5% anti-caking agent and 2.1-3% of the amount. 820A ensures that the agglomeration rate of DA-X citrate technical material is 0% at different temperatures, effectively preventing the agglomeration phenomenon of DA-X citrate technical material at high temperatures.

[0101] The clumping of DA-X citrate technical grade may be due to the citrate chelating onto the long chain of DA-X. At low temperatures, the chelating ability is strong, but as the temperature rises, the chelating ability decreases, the stability decreases, and clumping occurs.

[0102] The above-mentioned water content test results of DA-X citrate with a single anti-caking agent after being placed at different temperatures for a period of time are as follows: Figure 9 As shown, from Figure 9 It can be seen that the water content of DA-X citrate with a single anti-caking agent does not change much after being placed at different temperatures for a period of time. The difference in water content of the three DA-X citrate technical materials is determined by the water content of the initial technical material and is not affected by the introduced anti-caking agent.

[0103] (2) Agglomeration performance test under high humidity conditions

[0104] The caking rate of DA-X citrate technical grade with a single anti-caking agent at 25°C and an ambient temperature of 90% was tested as follows: Figure 10 As shown, Figure 10 The 5% anti-caking agent is 5% anti-caking agent 1, and the 5% anti-caking agent is anti-caking agent 2. The morphological changes of the original drug are as follows: Figure 11 As shown. From Figure 10-11 It can be seen that the effects of different anti-caking agents on the caking of DA-X citrate technical material vary greatly under 90% humidity conditions. Anti-caking agents 1, potassium pyrophosphate, nano-alumina, NT-104, AG, and 1% show significant differences. 22LS, 2% 22LS has virtually no anti-caking effect, but 3% of it... 22LS, 2% 820A, 3% 820A can effectively prevent caking, reducing the caking rate of DA-X citrate technical grade by up to 40%.

[0105] The moisture content test results of DA-X citrate technical grade with a single anti-caking agent at an ambient temperature of 90% are shown in Table 5. A bar chart of moisture content is plotted as follows. Figure 12 As shown, Figure 12 The 5% anti-caking agent is the same as the 5% anti-caking agent 1, and the 5% anti-caking agent is the same as the anti-caking agent 2.

[0106] Table 5. Water content of DA-X citrate at 90% ambient humidity.

[0107]

[0108]

[0109] From Table 5 and Figure 12 As can be seen, under 90% humidity conditions, the moisture content of DA-X citrate technical material after the introduction of the anti-caking agent is not significantly different, indicating that the addition of the anti-caking agent does not increase or decrease the hygroscopic properties of the technical material under 90% humidity conditions. The moisture content of DA-6 citrate technical material after the addition of... The humidity decreased slightly after 22LS, possibly because the addition of anti-caking agent reduced the material's moisture absorption performance.

[0110] 2. Anti-caking performance test of fatty acid diethylaminoethanol ester citrate technical material after being introduced into compound anti-caking agent

[0111] Based on the above tests on the caking performance of single anti-caking agents, 3% were selected. 22LS and 1% and 3% 820A was compounded with other anti-caking agents, and the composition of the compounded formulation is shown in Table 6.

[0112] Table 6. Formulation composition of DA-X citrate technical and compound anti-caking agent.

[0113]

[0114]

[0115] (1) Agglomeration performance test at different temperatures

[0116] The agglomeration rate test results of the above 39 formulations at different temperatures are shown in Tables 7-9.

[0117] Table 7. Agglomeration rate of DA-6 citrate with compound anti-caking agent introduced at different temperatures.

[0118]

[0119] Table 8. Agglomeration rate of DA-8 citrate with compound anti-caking agent introduced at different temperatures.

[0120]

[0121]

[0122] Table 9. Agglomeration rate of DA-10 citrate with compound anti-caking agent introduced at different temperatures.

[0123]

[0124] As can be seen from Table 7-9, except for formula #28 (which adds 4% of...) In addition to 22LS), the addition of anti-caking agents in other formulations can improve the anti-caking performance of DA-X citrate technical material at high temperatures. Compared with the addition of a single anti-caking agent, the combination with other anti-caking agents can better prevent the caking of DA-X citrate technical material. Under the conditions of 25℃-50℃, the caking rate is 0%, and no caking phenomenon occurs.

[0125] (2) Agglomeration performance test under high humidity conditions

[0126] The agglomeration rate of the above 39 formulations under the conditions of 25℃ and 90% ambient humidity is shown in Table 10.

[0127] Table 10 shows that, under 90% ambient humidity, the caking rates of formulations 3#-7# and 9#-13# in DA-6 citrate technical grade were lower than those of formulations 2# and 8#, respectively; the caking rates of formulations 16#-20# and 22#-26# in DA-8 citrate technical grade were lower than those of formulations 15# and 21#, respectively; and the caking rates of formulations 29#-33# and 35#-39# in DA-10 citrate technical grade were lower than those of formulations 28# and 34#, respectively. This indicates that compound anti-caking agents are more effective than single anti-caking agents in preventing caking of DA-X citrate technical grade. In the compound formulations, the caking rate of the SIPERNAT series combined with potassium pyrophosphate was higher than that of the SIPERNAT series combined with nano-alumina or NT-104.

[0128] In addition, DA-X citrate technical grade was added 820A (8#~13#), compared to adding 22LS (2#~7#) has a lower caking rate, reducing the caking rate of DA-X citrate technical grade to below 45%, indicating that... 820A can better improve the anti-caking properties of citrate technical.

[0129] Formula #5 (3%) 22LS and 1% potassium pyrophosphate compound) compared to formula #7 (2% potassium pyrophosphate compound) A mixture of 22LS and 2% potassium pyrophosphate showed a low agglomeration rate. DA-8 and DA-10 exhibited similar properties, indicating that the preferred mass ratio of silica powder to potassium pyrophosphate is 3:1. Formulation #12 (3% of...) The combination of 820A and 2% potassium pyrophosphate showed the lowest caking rate, indicating that the formulation has good anti-caking properties.

[0130] Table 10 Agglomeration rate of DA-X citrate with compound anti-caking agent under high humidity

[0131]

[0132] Based on the above screening test results, formulas 5#~7#, 11#~13#, 18#~20#, 24#~26#, 31#~33#, and 37#~39# were selected as preferred formulas, which are the fatty acid diethylaminoethanol ester citrate formulas of Examples 1 to 18 of the present invention.

[0133] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A fatty acid diethylaminoethanol ester citrate, characterized in that, It consists of fatty acid diethylaminoethanol ester citrate technical and 4-5% anti-caking agent, wherein the anti-caking agent is composed of silica powder and potassium pyrophosphate.

2. The fatty acid diethylaminoethanol ester citrate as described in claim 1, characterized in that, The mass ratio of silica powder to potassium pyrophosphate is 3:(1-3).

3. The fatty acid diethylaminoethanol ester citrate as described in claim 2, characterized in that, The mass ratio of silica powder to potassium pyrophosphate is 3:(1-2).

4. The fatty acid diethylaminoethanol ester citrate as described in claim 2, characterized in that, It consists of diethylaminoethanol fatty acid citrate technical and 5% anti-caking agent, wherein the mass ratio of silica powder to potassium pyrophosphate is 3:

2.

5. The fatty acid diethylaminoethanol ester citrate according to any one of claims 1-4, characterized in that, The fatty acid diethylaminoethanol ester citrate technical grade includes diethylaminoethanol hexanoate citrate technical grade, diethylaminoethanol octanoate citrate technical grade, and diethylaminoethanol decanoate citrate technical grade.

6. The fatty acid diethylaminoethanol ester citrate according to any one of claims 1-4, characterized in that, The silica powder was prepared by vapor deposition.

7. The fatty acid diethylaminoethanol ester citrate according to any one of claims 6, characterized in that, The particle size of the silica powder is 12 nm to 19 μm.

8. The fatty acid diethylaminoethanol ester citrate according to any one of claims 7, characterized in that, The particle size of the silica powder is 12-15 nm.

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