Composition for improving the stability and activity of sodium percarbonate, preparation method and application
By combining materials such as vapor phase silica and polyaniline and silane coupling agents, a covering network structure is formed, which solves the stability and activity of sodium percarbonate in complex environments, and improves its performance and market competitiveness in the fields of detergents, bleaches, disinfectants, etc.
Patent Information
- Application Number
- CN202510535408.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-27
- Publication Date
- 2025-08-15
- Estimated Expiration
- 2045-04-27
AI Technical Summary
The existing sodium percarbonate has insufficient stability and activity, which is susceptible to high temperature, humidity and heavy metal ions, resulting in a decline in performance in complex environments, and the traditional stabilizer contains phosphorus and is prone to environmental pollution.
The stabilizer is prepared by using inorganic materials such as vapor phase silica, polyaniline and specific silane coupling agents. By optimizing reaction conditions and spray drying process, a coating network structure is formed to isolate moisture and heavy metal ions, and the thermal stability and moisture stability of sodium percarbonate are improved.
It significantly enhances the stability and activity of sodium percarbonate, improves the application performance in detergents, bleaches, disinfectants and other fields, reduces production costs and expands the application scope.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of peroxides, and in particular to a composition for improving the stability and activity of sodium percarbonate, a preparation method and application thereof. Background Art
[0002] Sodium percarbonate is an important inorganic peroxide with the chemical formula 2Na2CO3·3H2O2 and a relative molecular mass of 314.0. It has bleaching, sterilization, degreasing, and cleaning properties, and is widely used in daily chemical products such as detergents, color-bleaching laundry detergents, toothpaste, and cosmetics. However, sodium percarbonate is chemically unstable and easily decomposes upon absorption of moisture, releasing reactive oxygen species and resulting in loss of its active ingredients. Therefore, stabilizers and additives are often added during the production process to enhance its stability.
[0003] Currently, sodium percarbonate is produced primarily through wet and dry processes. The wet process involves reacting sodium carbonate with hydrogen peroxide to produce sodium percarbonate. Stabilizers and additives are often added during the process to improve product quality. Traditional stabilizers, such as phosphates and their mixtures, and organophosphine additives, often contain phosphorus. While these substances can improve the stability of sodium percarbonate, phosphorus-containing formulations can easily lead to eutrophication of water bodies and cause environmental pollution. Therefore, the development of phosphorus-free stabilizers has become a research hotspot.
[0004] Chinese invention patent CN101391754A discloses a stabilizer for preparing phosphorus-free sodium percarbonate. The stabilizer is composed of the following components: a silicate, a copolymer of carboxylic acid and sulfonate, an inorganic magnesium salt, sodium polyacrylate, an organic alcoholamine, and disodium EDTA. The stabilizer is used by adding the silicate, the copolymer of carboxylic acid and sulfonate, and the inorganic magnesium salt to the sodium carbonate raw material, while the sodium polyacrylate, the organic alcoholamine, and disodium EDTA are added to the hydrogen peroxide raw material. The sodium percarbonate product prepared using this stabilizer has uniform particles with controllable particle size, an active oxygen content exceeding 13.8%, a bulk density exceeding 900 g / L, a thermal stability exceeding 85%, and a wet stability exceeding 55%. This stabilizer contains no phosphorus and can completely replace traditional phosphorus-containing formulations, reducing production costs and environmental pollution.
[0005] However, despite the excellent performance of this stabilizer in reducing environmental pollution, its stabilization ability and cleaning and washing effects in actual applications still need to be improved. For example, sodium percarbonate easily decomposes when exposed to high temperatures, water, or heavy metal ions, resulting in reduced active oxygen stability. In addition, small amounts of moisture or trace amounts of heavy metal ions such as iron, copper, and cobalt can accelerate its decomposition, affecting its application performance in complex environments. Therefore, developing a sodium percarbonate stabilizer with higher stability, better active oxygen retention ability, and better cleaning and washing effects is of great significance to improving the market competitiveness and application scope of sodium percarbonate products. Summary of the Invention
[0006] In order to address the deficiencies in the prior art, the present invention aims to provide a sodium percarbonate stabilizer with higher stability, better active oxygen retention capacity and better cleaning and washing effects.
[0007] In order to achieve the above-mentioned object of the invention, the present invention adopts the following technical solutions:
[0008] A method for preparing a composition for improving the stability and activity of sodium percarbonate is as follows, in parts by weight:
[0009] Step 1, adding 1-2 parts of sodium carbonate decahydrate and 0.5-2 parts of mother liquor into a slurry tank, heating to 25-35° C. and treating for 1-3 hours to obtain reaction solution A; adding 0.006-0.016 parts of crystallization aid A to 0.5-2 parts of hydrogen peroxide solution with a mass concentration of 25%-35%, stirring until completely dissolved, and cooling to 3-8° C. to obtain reaction solution B; adding 0.05-0.2 parts of crystallization aid B and 0.03-0.08 parts of stabilizer to 0.5-2 parts of water, stirring until completely dissolved, to obtain reaction solution C;
[0010] Step 2: Add 1 to 3 parts of the mother liquor as the base liquid to the reactor, control the reaction temperature at 15 to 25°C, add reaction liquid A, reaction liquid B and reaction liquid C to the reactor respectively, and react for 10 to 50 minutes. After the reaction is completed, stir at 800 to 1200 rpm for 3 to 8 minutes, and then immediately send it into a spray drying tower for spray drying to obtain the final composition.
[0011] The preparation method of the stabilizer is as follows, in parts by weight:
[0012] First, 100 to 150 parts of inorganic materials and 20 to 40 parts of functional agents are mixed, and then 1000 to 1500 parts of anhydrous ethanol, 5 to 10 parts of silane coupling agents and 2 to 6 parts of aluminum phosphate are added, mixed, and ultrasonically mixed and stirred. Subsequently, the mixture is treated at 60 to 70° C. for 30 to 50 minutes to obtain a stabilizer.
[0013] The temperature in the spray drying tower is 150-170° C., the vacuum degree is 15-25 kPa, and the residence time is 10-30 minutes.
[0014] The ultrasonic mixing and stirring is performed for 20 to 50 minutes, the ultrasonic power is 200 to 400 W, and the ultrasonic frequency is 20 to 60 kHz.
[0015] The mother liquor contains 6wt% to 8wt% of sodium carbonate, 0.5wt% to 1wt% of hydrogen peroxide, 14wt% to 28wt% of sodium sulfate and the balance is water.
[0016] The crystallization aid A is at least one of ethylenediaminetetraacetic acid, aminotrimethylenephosphonic acid, hydroxyethylenediphosphonic acid, sodium citrate, sodium polyacrylate, and diethylenetriaminepentamethylenephosphonic acid.
[0017] The crystallization aid B is at least one of sodium pyrophosphate, sodium tripolyphosphate, sodium hexametaphosphate, trisodium phosphate, disodium hydrogen phosphate, ammonium pyrophosphate, ethylenediaminetetramethylenephosphoric acid, and hydrolyzed polymaleic anhydride.
[0018] The inorganic material includes at least one of graphene, nano zinc oxide, and fumed silicon dioxide.
[0019] The functional agent is at least one of polyaniline, nano boron nitride and carbon nanotubes.
[0020] The silane coupling agent is at least one of N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea, 3-[tri(hexyloxy)silyl]propylamine, N-[3-[tri(octyloxy)silyl]propyl]ethylenediamine, and N-(2-aminoethyl)-3-aminopropyltrimethoxysilane.
[0021] The composition for improving the stability and activity of sodium percarbonate is applied in the fields of detergents, bleaches and disinfectants.
[0022] The creativity of the present invention lies in the development of an innovative sodium percarbonate stabilizer and its preparation method. In the preparation method of the stabilizer, a stabilizer prepared from an inorganic material, a functional agent, anhydrous ethanol, a silane coupling agent, and aluminum phosphate is used to improve the stability of the composition and the washing effect on clothes. In particular, the inorganic material is fumed silica, the functional agent is polyaniline, and the silane coupling agent is N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea, which has the best stability and washing effect. Fumed silica, with its high specific surface area and abundant surface hydroxyl groups, chemically bonds with N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea to form a coated network structure that effectively isolates moisture and heavy metal ions; polyaniline, due to its good electrical conductivity and chemical stability, forms a uniform coating on the surface of sodium percarbonate, further blocking decomposition factors. The stability and activity of sodium percarbonate are significantly improved, allowing it to maintain high performance even in complex environments. At the same time, the optimized spray drying process further improves the product's dispersion and particle uniformity. This innovative combination and process optimization not only breaks through the bottleneck of existing technologies, but also expands the application range of sodium percarbonate in detergents, bleaches, disinfectants and other fields, with significant market value and innovation.
[0023] In the present invention, the functions of each substance are as follows:
[0024] Sodium carbonate decahydrate is the main raw material of sodium percarbonate, providing carbonate ions , reacts with hydrogen peroxide to form sodium percarbonate.
[0025] The mother liquor provides the reaction medium, adjusts the pH value and ionic strength of the reaction system, and acts as a solvent to help dissolve sodium carbonate decahydrate.
[0026] Sodium sulfate acts as an electrolyte to adjust the ionic strength of the reaction system, improve the stability of the reaction, and prevent the decomposition of sodium percarbonate.
[0027] Sodium polyacrylate, as a crystallization aid, can regulate the crystallization process of sodium percarbonate and improve the particle size uniformity and particle strength of the product.
[0028] Diethylenetriaminepentamethylenephosphonic acid, as a crystallization aid, can chelate trace metal ions (such as iron, copper, manganese, etc.), prevent the decomposition of sodium percarbonate, and improve the stability of the product.
[0029] As a crystallization aid, trisodium phosphate can regulate the crystallization process of sodium percarbonate and improve the particle size uniformity and particle strength of the product.
[0030] The stabilizer isolates moisture and heavy metal ions through coating, significantly improving the thermal stability and wet stability of sodium percarbonate.
[0031] Fumed silica provides a high specific surface area and abundant surface hydroxyl groups, which can chemically bond with the silane coupling agent to form a stable network structure and enhance the coating effect of sodium percarbonate.
[0032] Polyaniline has good electrical conductivity and chemical stability, and can form a uniform coating on the surface of sodium percarbonate, effectively isolating moisture and heavy metal ions, and improving the thermal stability and wet stability of sodium percarbonate.
[0033] As a silane coupling agent, N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea can chemically bond with fumed silica and the like to form a stable network structure, further enhancing the coating effect of sodium percarbonate.
[0034] Aluminum phosphate enhances the structural stability of the stabilizer.
[0035] Anhydrous ethanol is used as a solvent to help the components of the stabilizer to be evenly dispersed and promote the chemical reaction.
[0036] The spray drying tower uses a spray drying process to quickly dry the reaction product to form a sodium percarbonate product with uniform particles, thereby improving the dispersibility and application performance of the product.
[0037] These substances significantly improve the stability and activity of sodium percarbonate through synergistic effects, enabling it to exhibit excellent performance in the fields of detergents, bleaches, and disinfectants.
[0038] Compared with the existing technology, it has the following beneficial effects:
[0039] 1) The stabilizer prepared by the present invention using materials such as fumed silica and polyaniline and a specific silane coupling agent (such as N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propylurea) effectively isolates decomposition factors such as moisture and heavy metal ions, significantly enhancing the thermal and wet stability of sodium percarbonate, allowing it to maintain a high active oxygen content even in high temperature and humid environments.
[0040] 2) This invention further improves the dispersibility and particle uniformity of sodium percarbonate by optimizing reaction conditions (such as temperature, stirring speed, and reaction time) and the spray drying process. This optimized process not only improves product quality but also reduces production costs and increases production efficiency.
[0041] 3) The sodium percarbonate composition prepared by the present invention exhibits excellent performance in multiple fields such as detergents, bleaches, and disinfectants, and has broad application prospects and market value. DETAILED DESCRIPTION
[0042] Main sources of substances:
[0043] Fumed silica, specification: DM-20S, product specification: 12nm, manufacturer (origin): Tokuyama, Japan.
[0044] Polyaniline, product number: PA05600, Guangdong Wengjiang Chemical Reagent Co., Ltd.
[0045] Sodium polyacrylate, product number: 391, Jiangsu Caiwei Biotechnology Co., Ltd.
[0046] Nano boron nitride, product number: PT-BN-100nm, particle size: 100nm, specific surface area: 19m 2 / g, Shanghai Pantian Powder Materials Co., Ltd.
[0047] Nano zinc oxide, model: KND-XR30, particle size: 30-50 nm, Changzhou Konada New Material Technology Co., Ltd.
[0048] Graphene, item number: NO-C-066-2, diameter <10um, surface area: 300-350m 2 / g, Shanghai Naionano Technology Co., Ltd.
[0049] Carbon nanotubes, model: KR-30A, fineness: 8-15nm, Kerri Nano (Guangdong) Co., Ltd.
[0050] Hydrolyzed polymaleic anhydride, product number: HPMA, Dezhou Chengqi Chemical Co., Ltd.
[0051] The remaining raw materials in the examples and comparative examples of the present invention are all commercially available products.
[0052] The design concept of this invention is to improve the stability and activity of sodium percarbonate by preparing a special stabilizer. This stabilizer is composed of a mixture of inorganic materials such as fumed silica and polyaniline, and an organosilane coupling agent (such as N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propylurea). Its coating effect effectively isolates the sodium percarbonate from decomposition factors such as moisture and heavy metal ions, while also enhancing its thermal and wet stability. Furthermore, by optimizing the reaction conditions and spray drying process, the dispersibility and application properties of sodium percarbonate are further improved, resulting in excellent performance in detergents, bleaches, and disinfectants.
[0053] Example 1
[0054] A method for preparing a composition for improving the stability and activity of sodium percarbonate is as follows:
[0055] Step 1: 1.5 kg of sodium carbonate decahydrate and 1 kg of mother liquor are added to a slurry tank, wherein the mother liquor contains 6 wt% of sodium carbonate, 0.8 wt% of hydrogen peroxide, 20 wt% of sodium sulfate, and the balance is water, and the temperature is raised to 30° C. for 2 hours to obtain reaction solution A; 5 g of sodium polyacrylate and 5 g of diethylenetriamine penta methylenephosphonic acid are added to 1 kg of 35% hydrogen peroxide solution, stirred until completely dissolved, and cooled to 5° C. to obtain reaction solution B; 100 g of trisodium phosphate and 50 g of stabilizer are added to 1 kg of water, stirred until completely dissolved, to obtain reaction solution C;
[0056] Step 2: Add 2 kg of mother liquor as a bottom liquid to the reactor, wherein the mother liquor contains 6 wt% sodium carbonate, 0.8 wt% hydrogen peroxide, 20 wt% sodium sulfate, and the balance is water. The reaction temperature is controlled at 20 ° C. Reaction liquid A, reaction liquid B, and reaction liquid C are added to the reactor respectively. The reaction time is 30 minutes. After the reaction is completed, stir at 1000 rpm for 5 minutes, and then immediately send it to a spray drying tower for spray drying. The temperature in the spray drying tower is 160 ° C, the vacuum degree is 20 kPa, and it stays for 20 minutes to obtain the final composition.
[0057] The preparation method of the stabilizer is as follows:
[0058] First, 120 g of fumed silica and 30 g of polyaniline were mixed, followed by the addition of 1200 g of anhydrous ethanol, 8 g of N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea and 4 g of aluminum phosphate, and the mixture was ultrasonically stirred for 40 minutes at an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, followed by treatment at 65 ° C for 45 minutes to obtain a stabilizer.
[0059] Example 2
[0060] A method for preparing a composition for improving the stability and activity of sodium percarbonate is as follows:
[0061] Step 1: 1.5 kg of sodium carbonate decahydrate and 1 kg of mother liquor are added to a slurry tank, wherein the mother liquor contains 6 wt% of sodium carbonate, 0.8 wt% of hydrogen peroxide, 20 wt% of sodium sulfate, and the balance is water, and the temperature is raised to 30° C. for 2 hours to obtain reaction solution A; 5 g of sodium polyacrylate and 5 g of diethylenetriamine penta methylenephosphonic acid are added to 1 kg of 35% hydrogen peroxide solution, stirred until completely dissolved, and cooled to 5° C. to obtain reaction solution B; 100 g of hydrolyzed polymaleic anhydride and 50 g of stabilizer are added to 1 kg of water, stirred until completely dissolved, to obtain reaction solution C;
[0062] Step 2: Add 2 kg of mother liquor as a bottom liquid to the reactor, wherein the mother liquor contains 6 wt% sodium carbonate, 0.8 wt% hydrogen peroxide, 20 wt% sodium sulfate, and the balance is water. The reaction temperature is controlled at 20 ° C. Reaction liquid A, reaction liquid B, and reaction liquid C are added to the reactor respectively. The reaction time is 30 minutes. After the reaction is completed, stir at 1000 rpm for 5 minutes, and then immediately send it to a spray drying tower for spray drying. The temperature in the spray drying tower is 160 ° C, the vacuum degree is 20 kPa, and it stays for 20 minutes to obtain the final composition.
[0063] The preparation method of the stabilizer is the same as that in Example 1.
[0064] Example 3
[0065] The preparation method of a composition for improving the stability and activity of sodium percarbonate is basically the same as that of Example 1, the only difference being the preparation method of the stabilizer.
[0066] The preparation method of the stabilizer is as follows:
[0067] First, 120g of nano-zinc oxide and 30g of polyaniline were mixed, and then 1200g of anhydrous ethanol, 8g of N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea and 4g of aluminum phosphate were added and mixed. The mixture was ultrasonically stirred for 40 minutes at an ultrasonic power of 300W and an ultrasonic frequency of 40kHz, and then treated at 65°C for 45 minutes to obtain a stabilizer.
[0068] Example 4
[0069] The preparation method of a composition for improving the stability and activity of sodium percarbonate is basically the same as that of Example 1, the only difference being the preparation method of the stabilizer.
[0070] The preparation method of the stabilizer is as follows:
[0071] First, 120 g of fumed silica and 30 g of nano-boron nitride were mixed, followed by the addition of 1200 g of anhydrous ethanol, 8 g of N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea and 4 g of aluminum phosphate. The mixture was ultrasonically stirred for 40 minutes at an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, and then treated at 65°C for 45 minutes to obtain a stabilizer.
[0072] Example 5
[0073] The preparation method of a composition for improving the stability and activity of sodium percarbonate is basically the same as that of Example 1, the only difference being the preparation method of the stabilizer.
[0074] The preparation method of the stabilizer is as follows:
[0075] First, 120 g of fumed silica and 30 g of polyaniline were mixed, followed by the addition of 1200 g of anhydrous ethanol, 8 g of 3-[tri(hexyloxy)silyl]propylamine, and 4 g of aluminum phosphate. The mixture was ultrasonically stirred for 40 minutes at an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, and then treated at 65° C. for 45 minutes to obtain a stabilizer.
[0076] Example 6
[0077] The preparation method of a composition for improving the stability and activity of sodium percarbonate is basically the same as that of Example 1, the only difference being the preparation method of the stabilizer.
[0078] The preparation method of the stabilizer is as follows:
[0079] First, 120 g of fumed silica and 30 g of polyaniline were mixed, followed by the addition of 1200 g of anhydrous ethanol, 8 g of N-[3-[tri(octyloxy)silyl]propyl]ethylenediamine and 4 g of aluminum phosphate, and the mixture was ultrasonically stirred for 40 minutes at an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, followed by treatment at 65° C. for 45 minutes to obtain a stabilizer.
[0080] Example 7
[0081] The preparation method of a composition for improving the stability and activity of sodium percarbonate is basically the same as that of Example 1, the only difference being the preparation method of the stabilizer.
[0082] The preparation method of the stabilizer is as follows:
[0083] First, 120 g of graphene and 30 g of polyaniline were mixed, followed by the addition of 1200 g of anhydrous ethanol, 8 g of N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea and 4 g of aluminum phosphate, and the mixture was ultrasonically stirred for 40 minutes at an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz, followed by treatment at 65 ° C for 45 minutes to obtain a stabilizer.
[0084] Example 8
[0085] The preparation method of a composition for improving the stability and activity of sodium percarbonate is basically the same as that of Example 1, the only difference being the preparation method of the stabilizer.
[0086] The preparation method of the stabilizer is as follows:
[0087] First, 120 g of fumed silica and 30 g of carbon nanotubes were mixed, followed by the addition of 1200 g of anhydrous ethanol, 8 g of N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propylurea and 4 g of aluminum phosphate, and the mixture was ultrasonically stirred for 40 minutes at an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz. The mixture was then treated at 65 ° C for 45 minutes to obtain a stabilizer.
[0088] Example 9
[0089] The preparation method of a composition for improving the stability and activity of sodium percarbonate is basically the same as that of Example 1, the only difference being the preparation method of the stabilizer.
[0090] The preparation method of the stabilizer is as follows:
[0091] First, 120 g of fumed silica and 30 g of polyaniline were mixed, followed by the addition of 1200 g of anhydrous ethanol, 8 g of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 4 g of aluminum phosphate, and the mixture was ultrasonically stirred for 40 minutes at an ultrasonic power of 300 W and an ultrasonic frequency of 40 kHz. The mixture was then treated at 65°C for 45 minutes to obtain a stabilizer.
[0092] Example 10
[0093] A method for preparing a composition for improving the stability and activity of sodium percarbonate is as follows:
[0094] Step 1: 1.5 kg of sodium carbonate decahydrate and 1 kg of mother liquor are added to a slurry tank, wherein the mother liquor contains 6 wt% of sodium carbonate, 0.8 wt% of hydrogen peroxide, 20 wt% of sodium sulfate, and the balance is water, and the temperature is raised to 30° C. for 2 hours to obtain reaction solution A; 5 g of sodium polyacrylate and 5 g of diethylenetriaminepentamethylenephosphonic acid are added to 1 kg of 35% hydrogen peroxide solution, stirred until completely dissolved, and cooled to 5° C. to obtain reaction solution B; 100 g of ethylenediaminetetramethylenephosphonic acid and 50 g of stabilizer are added to 1 kg of water, stirred until completely dissolved, to obtain reaction solution C;
[0095] Step 2: Add 2 kg of mother liquor as a bottom liquid to the reactor, wherein the mother liquor contains 6 wt% sodium carbonate, 0.8 wt% hydrogen peroxide, 20 wt% sodium sulfate, and the balance is water. The reaction temperature is controlled at 20 ° C. Reaction liquid A, reaction liquid B, and reaction liquid C are added to the reactor respectively. The reaction time is 30 minutes. After the reaction is completed, stir at 1000 rpm for 5 minutes, and then immediately send it to a spray drying tower for spray drying. The temperature in the spray drying tower is 160 ° C, the vacuum degree is 20 kPa, and it stays for 20 minutes to obtain the final composition.
[0096] The preparation method of the stabilizer is the same as that in Example 1.
[0097] Comparative Example 1
[0098] A method for preparing a composition for improving the stability and activity of sodium percarbonate is as follows:
[0099] Step 1: 1.5 kg of sodium carbonate decahydrate and 1 kg of mother liquor are added to a slurry tank, wherein the mother liquor contains 6% sodium carbonate, 0.8% hydrogen peroxide, 20% sodium sulfate, and the balance is water, and the temperature is raised to 30° C. for 2 hours to obtain reaction solution A; 5 g of sodium polyacrylate and 5 g of diethylenetriamine penta-methylenephosphonic acid are added to 1 kg of 35% hydrogen peroxide solution, stirred until completely dissolved, and cooled to 5° C. to obtain reaction solution B; 100 g of trisodium phosphate is added to 1 kg of water and stirred until completely dissolved to obtain reaction solution C;
[0100] Step 2: Add 2 kg of mother liquor as a bottom liquid to the reactor, wherein the mother liquor contains 6% sodium carbonate, 0.8% hydrogen peroxide, 20% sodium sulfate, and the balance is water. The reaction temperature is controlled at 20 ° C. Reaction liquid A, reaction liquid B, and reaction liquid C are added to the reactor respectively. The reaction time is 30 minutes. After the reaction is completed, stir at 1000 rpm for 5 minutes, and then immediately send it to a spray drying tower for spray drying. The temperature in the spray drying tower is 160 ° C, the vacuum degree is 20 kPa, and it stays for 20 minutes to obtain the final composition.
[0101] Test Example 1
[0102] Stability performance test
[0103] The composition prepared in the present invention was subjected to thermal stability and moisture stability tests (test standard: "HG / T 2764-2013 Industrial Sodium Percarbonate"). Specific test data are shown in Table 1.
[0104] Table 1
[0105]
[0106] Test Example 2
[0107] Washing effect test
[0108] The composition prepared by the present invention is added to a commercially available liquid detergent at a mass fraction of 1% of the detergent for use. During the washing process, the protected sodium percarbonate is released, thereby achieving the washing or bleaching function.
[0109] Evaluation of washing performance: 36 items of clothing, similar in condition, soiling, and size, were selected and divided into 9 groups of 4 items each. Each group was then washed using the composition prepared by the present invention. Machine washing was performed, and the cleaning performance was recorded. Cleaning performance was evaluated on a scale of 0-10, with 0 representing very poor and 10 representing very good. Deodorization performance was evaluated on a scale of 0-10, with 0 representing very poor and 10 representing very good. The average values were calculated, and the test results are shown in Table 2.
[0110] Table 2
[0111]
[0112] From the data of test examples 1 to 2, it can be seen that the composition prepared in Example 1 has the best stability and washing effect on clothes compared with the composition prepared in Examples 3 to 10.
[0113] Sodium percarbonate, due to its unstable chemical properties, is prone to decomposition at high temperatures, in contact with water, or when exposed to heavy metal ions, resulting in reduced active oxygen stability. The present invention prepares a stabilizer by mixing fumed silica and polyaniline, then adding anhydrous ethanol, N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea, and aluminum phosphate. This stabilizer effectively isolates moisture and heavy metal ions through its coating effect, significantly improving the stability and dispersibility of sodium percarbonate and enhancing its application performance in complex environments.
[0114] The stabilizer prepared using fumed silica in Example 1 exhibited superior stability and washing effects, primarily due to the unique physicochemical properties of fumed silica. Fumed silica has an extremely high specific surface area and abundant surface hydroxyl groups, which can chemically bond with silane coupling agents (such as N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea) to form a stable network structure, thereby effectively coating the sodium percarbonate particles and enhancing their thermal and wet stability. In addition, the nanoscale particle size and good dispersibility of fumed silica enable it to be evenly distributed on the surface of sodium percarbonate, further improving the dispersibility and decomposition resistance of sodium percarbonate. It exhibits good dispersibility in the detergent system, effectively reducing surface tension, enhancing foam stability, and thus improving the washing effect. In contrast, although nano zinc oxide has certain chemical stability, its surface activity and coating effect are inferior to those of fumed silica; although graphene has excellent conductivity and specific surface area, its dispersibility and stability in water are poor, and it easily agglomerates, resulting in poor coating effect. Therefore, the use of fumed silica in Example 1 significantly improved the stability and washing effect of sodium percarbonate, making it perform best in all tests.
[0115] In Example 1, polyaniline is used as a component of the stabilizer, which shows better stability and washing effect than nano-boron nitride and carbon nanotubes. This is mainly attributed to the chemical and physical properties of polyaniline. Polyaniline has good electrical conductivity and chemical stability, and can form a uniform coating layer on the surface of sodium percarbonate, effectively isolating decomposition factors such as moisture and heavy metal ions, thereby significantly improving the thermal stability and wet stability of sodium percarbonate. In addition, the high specific surface area and porous structure of polyaniline enable it to better adsorb and disperse stains during the washing process, thereby improving the washing effect. In contrast, although nano-boron nitride has good thermal conductivity and chemical stability, its coating effect and adsorption capacity are not as good as polyaniline; carbon nanotubes are easy to agglomerate and have poor dispersibility, resulting in poor performance in stability and washing effect. Therefore, polyaniline, as a key component of the stabilizer in the present invention, significantly improves the comprehensive performance of sodium percarbonate.
[0116] The N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea used in Example 1 is used as a silane coupling agent. Compared with the different silane coupling agents used in other embodiments and comparative examples, it shows more excellent stability and washing effect. This is mainly due to its unique chemical structure and reaction characteristics. N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea contains two different siloxane groups, which can form a more stable chemical bond with fumed silica, thereby constructing a more dense and uniform coating. This coating can not only effectively isolate decomposition factors such as moisture and heavy metal ions, but also enhance the thermal stability and wet stability of sodium percarbonate. In comparison, while other silane coupling agents (such as 3-[tri(hexyloxy)silyl]propylamine, N-[3-[tri(octyloxy)silyl]propyl]ethylenediamine, and N-(2-aminoethyl)-3-aminopropyltrimethoxysilane) can also provide a certain stabilizing effect, their chemical bonding ability and coating effect are inferior to N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea, resulting in slightly inferior performance in terms of stability and cleaning effect. Therefore, N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propionurea used in Example 1 performed the best in improving the overall performance of sodium percarbonate.
[0117] In Example 2, hydrolyzed polymaleic anhydride (HPMA) was used as a crystallization aid, demonstrating superior stability and cleaning performance compared to diethylenetriaminepentamethylenephosphonic acid (DTPA) in Example 1 and ethylenediaminetetramethylenephosphonic acid (EDTA) in Example 10. Hydrolyzed PMA has a highly polymerized carboxyl structure, which can form stable chelates with metal ions (such as calcium, magnesium, and iron) in sodium percarbonate, effectively inhibiting the catalytic effect of these ions on the decomposition of SPC. Furthermore, the polymeric structure of HPMA enables improved dispersibility and uniformity in solution, forming a denser protective layer on the SPC surface, further enhancing its thermal and wet stability. During the washing process, the high molecular weight and linear structure of HPMA enable better stain dispersion, improving washing efficiency and deodorizing performance. Therefore, HPMA excels in enhancing the stability and cleaning performance of SPC.
Claims
1. A method for preparing a composition for improving the stability and activity of sodium percarbonate, characterized in that: The method is as follows, in parts by weight: Step 1, adding 1-2 parts of sodium carbonate decahydrate and 0.5-2 parts of mother liquor into a slurry tank, heating to 25-35° C. and treating for 1-3 hours to obtain reaction solution A; adding 0.006-0.016 parts of crystallization aid A to 0.5-2 parts of hydrogen peroxide solution with a mass concentration of 25%-35%, stirring until completely dissolved, and cooling to 3-8° C. to obtain reaction solution B; adding 0.05-0.2 parts of crystallization aid B and 0.03-0.08 parts of stabilizer to 0.5-2 parts of water, stirring until completely dissolved, to obtain reaction solution C; Step 2: Add 1 to 3 parts of the mother liquor as a base liquid to the reactor, control the reaction temperature at 15 to 25° C., add reaction solution A, reaction solution B, and reaction solution C to the reactor respectively, and react for 10 to 50 minutes. After the reaction is completed, stir at 800 to 1200 rpm for 3 to 8 minutes, and then immediately send the mixture into a spray drying tower for spray drying to obtain the final composition; The crystallization aid A is at least one of ethylenediaminetetraacetic acid, aminotrimethylenephosphonic acid, hydroxyethylenediphosphonic acid, sodium citrate, sodium polyacrylate, and diethylenetriaminepentamethylenephosphonic acid; The crystallization aid B is hydrolyzed polymaleic anhydride; The preparation method of the stabilizer is as follows, in parts by weight: First, 100-150 parts of inorganic material and 20-40 parts of functional agent are mixed, and then 1000-1500 parts of anhydrous ethanol, 5-10 parts of silane coupling agent and 2-6 parts of aluminum phosphate are added, mixed, and ultrasonically mixed and stirred, and then treated at 60-70°C for 30-50 minutes to obtain a stabilizer; The inorganic material is fumed silica; The functional agent is polyaniline; The silane coupling agent is N-3-(triethoxysilyl)propyl-N-3-(trimethoxysilyl)propylurea.
2. the preparation method of the composition that improves sodium percarbonate stability and activity as claimed in claim 1, is characterized in that, The temperature in the spray drying tower is 150-170° C., the vacuum degree is 15-25 kPa, and the residence time is 10-30 minutes.
3. the preparation method of the composition that improves sodium percarbonate stability and activity as claimed in claim 1, is characterized in that, The mother liquor contains 6wt% to 8wt% of sodium carbonate, 0.5wt% to 1wt% of hydrogen peroxide, 14wt% to 28wt% of sodium sulfate and the balance is water.
4. the preparation method of the composition that improves sodium percarbonate stability and activity as claimed in claim 1, is characterized in that, The ultrasonic mixing and stirring is performed for 20 to 50 minutes, the ultrasonic power is 200 to 400 W, and the ultrasonic frequency is 20 to 60 kHz.
5. A composition for improving the stability and activity of sodium percarbonate, characterized in that: The method is prepared by any one of claims 1 to 4.
6. An application of a composition for improving the stability and activity of sodium percarbonate as claimed in claim 5, characterized in that: Used in the industrial cleaning fields of detergents, bleaches and disinfectants.
Citation Information
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