Aluminum lactate powder as well as preparation method and application thereof

Abstract

The invention relates to the technical field of preparation of aluminum-containing powder, in particular to aluminum lactate powder as well as a preparation method and application thereof. The preparation method comprises the following steps: carrying out a neutralization reaction on a lactic acid solution and amorphous aluminum hydroxide to obtain aluminum lactate slurry; drying the aluminum lactate slurry to obtain an aluminum lactate powder product; the preparation method of the amorphous aluminum hydroxide comprises the following steps: carrying out first stirring on a soluble salt containing bicarbonate radicals and a solvent to obtain a bicarbonate solution; carrying out double hydrolysis reaction on the aluminate-containing solution, amorphous aluminum hydroxide seed crystals and a hydrogen carbonate solution to obtain an amorphous aluminum hydroxide wet material; and drying the amorphous aluminum hydroxide wet material to obtain the amorphous aluminum hydroxide. According to the preparation method, traditional common aluminum hydroxide is replaced with amorphous aluminum hydroxide, the reaction efficiency of the aluminum hydroxide and lactic acid can be improved, the time needed for preparing the aluminum lactate powder is shortened to 0.5 h or below, and the prepared aluminum lactate powder product is high in purity.

Description

Technical Field

[0001] The present application relates to the technical field of aluminum-containing powder preparation, and in particular to an aluminum lactate powder and a preparation method and application thereof. Background Art

[0002] Aluminum lactate is an inorganic aluminum compound with a molecular formula of C9H 15 AlO9, currently aluminum lactate is an important daily chemical reagent, and has been widely used in toothpaste, cosmetics and detergents. Aluminum lactate is mainly used as a stabilizer, sterilizer and astringent in toothpaste. In cosmetics, aluminum lactate plays a role in stabilizing and moisturizing, which can prevent the precipitation and stratification of cosmetics and affect their use effect. In addition, in the medical field, aluminum lactate can be used for astringent hemostasis, sterilization and other aspects.

[0003] At present, the preparation method of aluminum lactate is mainly divided into three categories: metal aluminum and lactic acid reaction, aluminum hydroxide and lactic acid reaction, and aluminum salt and lactic acid reaction. In the process of aluminum hydroxide and lactic acid reaction, based on the weak acidity of lactic acid, the process of the reaction is particularly slow, so it is necessary to carry out under heating conditions, and the slow reaction process causes the heating time of the reaction to be too long, which may lead to low yield of aluminum lactate. In addition, the reaction time of metal aluminum and lactic acid will also be longer, which makes this process also need to be continuously heated to speed up the reaction, and the continuous heating method will cause the energy consumption of the method to be high, and the reaction of metal aluminum and lactic acid also needs to be carried out under the catalytic action of a catalyst, and the use of a catalyst will seriously pollute the environment; in addition, the process of aluminum salt and lactic acid reaction does not require the catalytic action of a catalyst, and the reaction rate is faster, but the use amount of aluminum salt is large and the cost is high, and impurities are easily introduced during the reaction so that the purity of the aluminum lactate powder product obtained by the reaction cannot be guaranteed. Therefore, considering comprehensively, it is the best choice to use aluminum hydroxide and lactic acid reaction at this stage, but the efficiency of the reaction is low. Summary of the invention

[0004] The present application provides an aluminum lactate powder and a preparation method and application thereof to solve the following technical problem: how to improve the reaction efficiency of the reaction between aluminum hydroxide and lactic acid.

[0005] In a first aspect, the present application provides a method for preparing aluminum lactate powder, the preparation method comprising:

[0006] The lactic acid solution and amorphous aluminum hydroxide are neutralized to obtain aluminum lactate slurry.

[0007] Drying the aluminum lactate slurry to obtain an aluminum lactate powder product;

[0008] Wherein, the preparation method of the amorphous aluminum hydroxide comprises:

[0009] A soluble salt containing bicarbonate is first stirred with a solvent to obtain a bicarbonate solution;

[0010] Aluminate solution, amorphous aluminum hydroxide seed crystals and the bicarbonate solution are subjected to a double hydrolysis reaction to obtain amorphous aluminum hydroxide crystals;

[0011] The amorphous aluminum hydroxide crystals are dried to obtain amorphous aluminum hydroxide.

[0012] Optionally, the neutralization reaction temperature is 35°C to 60°C, and the neutralization reaction time is 30min to 75min; and / or

[0013] The neutralization reaction is carried out under the second stirring condition, and the rotation speed of the second stirring is ≥350r / min.

[0014] Optionally, the lactic acid solution comprises a lactic acid solute and a hydrophilic solvent, and the weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m1:m2=1:(0.24-0.67); and / or

[0015] The weight m3 of the hydrophilic solvent and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m3:m2=1:(0.12-0.59).

[0016] Optionally, the temperature of the double hydrolysis reaction is ≤60°C, the time of the double hydrolysis reaction is 3h to 6h, and the pH of the double hydrolysis reaction is 12.0 to 13.5.

[0017] Optionally, the drying temperature is 110° C. to 150° C., and the drying time is 50 min to 120 min; and / or

[0018] The temperature of the drying treatment is 60° C. to 80° C., and the time of the drying treatment is 0.5 h to 1.5 h.

[0019] Optionally, the mass concentration of aluminum oxide in the aluminate-containing solution is 35 g / L to 79 g / L; and / or

[0020] The added amount m4 of the amorphous aluminum hydroxide seed crystals and the weight m5 of the aluminum oxide in the aluminate solution satisfy the relationship: m4:m5=(1-5):100.

[0021] Optionally, the first stirring speed is ≥600r / min; and / or

[0022] The mass concentration of bicarbonate in the bicarbonate solution is 36.75 g / L to 94.8 g / L; and / or

[0023] The bicarbonate solution includes at least one of the following: sodium bicarbonate, potassium bicarbonate and ammonium bicarbonate.

[0024] In a second aspect, the present application provides an aluminum lactate powder, which is obtained by the preparation method described in the first aspect.

[0025] In a third aspect, the present application provides a binder, which includes the aluminum lactate powder described in the second aspect.

[0026] In a fourth aspect, the present application provides a method for preparing the adhesive according to the third aspect, the method comprising:

[0027] Mixing aluminum powder, magnesium powder and the aluminum lactate powder to obtain a mixed powder;

[0028] The mixed powder is ground to obtain an aluminum lactate adhesive; wherein the weight m6 of the aluminum powder, the weight m7 of the magnesium powder and the weight m8 of the aluminum lactate powder satisfy the relationship: m6:m7:m8=(4-12):(10-18):(70-86).

[0029] The above technical solution provided by the embodiment of the present application has the following advantages compared with the prior art:

[0030] The present application provides a method for preparing aluminum lactate powder. The method firstly obtains an amorphous aluminum hydroxide product having a large amount of disordered structure through a double hydrolysis reaction of a bicarbonate solution, an aluminate solution and an amorphous aluminum hydroxide seed crystal, so that the structure of the amorphous aluminum hydroxide is looser than that of traditional aluminum hydroxide crystals. The amorphous aluminum hydroxide with a looser structure has complex surface binding sites. When replacing traditional aluminum hydroxide crystals to react with lactic acid, lactic acid molecules will enter the structure of the amorphous aluminum hydroxide in large quantities and combine with these complex surface binding sites, thereby improving the reaction efficiency of the reaction between aluminum hydroxide and lactic acid. In addition, the amorphous aluminum hydroxide with complex surface binding sites can also improve the morphology of the generated aluminum lactate powder and avoid agglomeration between aluminum lactate powders, thereby improving the fluidity and dispersibility of the aluminum lactate powder, accelerating the neutralization reaction, and ultimately improving the reaction efficiency of the reaction between aluminum hydroxide and lactic acid. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and, together with the description, serve to explain the principles of the present application.

[0032] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.

[0033] Figure 1 A schematic diagram of a process for preparing aluminum lactate powder provided in an embodiment of the present application;

[0034] Figure 2 A schematic flow chart of a method for preparing an adhesive provided in an embodiment of the present application. DETAILED DESCRIPTION

[0035] In order to make the purpose, technical solution and advantages of the embodiments of the present application clearer, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application.

[0036] Various embodiments of the present application may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity and should not be understood as a rigid limitation on the scope of the present application; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single numerical values ​​within the range; for example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which applies regardless of the range; in addition, whenever a numerical range is indicated in this document, it is meant to include any cited numbers (fractions or integers) within the indicated range.

[0037] In this document, the terms including "including" and "including" mean "including but not limited to". Relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. "And / or" describes the association relationship of associated objects, indicating that there can be three relationships. For example, A and / or B can mean: A exists alone, A and B exist at the same time, and B exists alone; where A and B can be singular or plural. "At least one" means one or more, and "plurality" means two or more; "at least one", "at least one of the following" or similar expressions, refers to any combination of these items, including any combination of single or plural items; for example, "at least one of a, b, or c", or "at least one of a, b, and c" can all mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple. "Parts" such as parts by weight and parts by mass indicate the proportional relationship between the components. In the proportional relationship involved in this article, the parameters that need to be described by proportion should be understood as the first term of the proportional formula in the order of description, and the proportional numbers should be understood as the second term of the proportional formula. For example, if the mass ratio of substance A, substance B and substance C is 1:2:3, then substance A, substance B and substance C should correspond to the proportional numbers in the proportional formula in the order of description, that is, the mass of substance A: the mass of substance B: the mass of substance C = 1:2:3.

[0038] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in this article can be purchased from the market or prepared by existing methods.

[0039] Figure 1 A schematic diagram of a process for preparing aluminum lactate powder provided in an embodiment of the present application is exemplarily shown;

[0040] Figure 1 As shown, the present application embodiment provides a method for preparing aluminum lactate powder, the preparation method comprising:

[0041] S1. neutralizing the lactic acid solution and amorphous aluminum hydroxide to obtain an aluminum lactate slurry;

[0042] S2. Drying the aluminum lactate slurry to obtain an aluminum lactate powder product; wherein the preparation method of the amorphous aluminum hydroxide comprises:

[0043] S101. A soluble salt containing bicarbonate is first stirred with a solvent to obtain a bicarbonate solution;

[0044] S102. Aluminate solution, amorphous aluminum hydroxide seed crystals and the bicarbonate solution are subjected to a double hydrolysis reaction to obtain amorphous aluminum hydroxide wet material;

[0045] S103. Drying the wet amorphous aluminum hydroxide to obtain amorphous aluminum hydroxide.

[0046] It should be noted that the amorphous aluminum hydroxide does not have a clear crystalline form and is a non-crystalline substance. The amorphous structure of amorphous aluminum hydroxide is formed by the arrangement of hydroxide ions and aluminum ions in an amorphous arrangement. This arrangement determines that the structure of amorphous aluminum hydroxide is looser than that of traditional aluminum hydroxide crystals, and makes the amorphous aluminum hydroxide have a hyperbolic shape and a huge specific surface area. This morphology makes the amorphous aluminum hydroxide have physical properties that are completely different from the crystal structure, so as to improve the surface activity of amorphous aluminum hydroxide, thereby improving the reaction efficiency of the reaction between amorphous aluminum hydroxide and lactic acid.

[0047] It should be noted that the lactic acid solution is a lactic acid solution formed by dissolving lactic acid in deionized water.

[0048] It should be noted that the drying process can be performed by microwave drying.

[0049] It should be noted that an acid-base regulator can be added during the double hydrolysis reaction to maintain the pH of the double hydrolysis reaction at a preset pH level, thereby promoting the double hydrolysis reaction to proceed fully and quickly; the acid-base regulator can be sodium bicarbonate, sodium hydroxide, ammonia water, potassium hydroxide, or sodium aluminate.

[0050] In some optional embodiments, the temperature of the neutralization reaction is 35°C to 60°C, and the time of the neutralization reaction is 30min to 75min; and / or

[0051] The neutralization reaction is carried out under a second stirring condition, wherein the second stirring speed is ≥350 r / min;

[0052] In these embodiments, the temperature of the neutralization reaction can be 35°C to 60°C, and the time of the neutralization reaction can be 30min to 75min, so that the lactic acid solute in the lactic acid solution and the amorphous aluminum hydroxide can fully undergo a neutralization reaction under relatively low temperature conditions to accelerate the neutralization reaction, thereby ultimately improving the reaction efficiency of the reaction between aluminum hydroxide and lactic acid; in addition, the neutralization reaction can include a neutralization reaction under a preset stirring speed condition, and a preset stirring speed of ≥350r / min, so as to promote the neutralization reaction under a faster stirring speed condition, so as to promote the amorphous aluminum hydroxide and lactic acid to fully undergo a neutralization reaction and generate an aluminum lactate slurry containing a large amount of aluminum lactate.

[0053] The temperature of the neutralization reaction may be 35°C, 40°C, 45°C, 50°C, 55°C or 60°C.

[0054] The neutralization reaction time can be 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, 65 min, 70 min or 75 min.

[0055] In some optional embodiments, the lactic acid solution comprises a lactic acid solute and a hydrophilic solvent, and the weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m1:m2=1:(0.24-0.67); and / or

[0056] The weight m3 of the hydrophilic solvent and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m3:m2=1:(0.12-0.59).

[0057] In these embodiments, the lactic acid solution may include lactic acid solute, and the weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide may satisfy the relationship: m1:m2=1:(0.24-0.67), so that the neutralization reaction has a sufficient amount of amorphous aluminum hydroxide, and the sufficient amount of amorphous aluminum hydroxide can quickly and fully react with the lactic acid solute to improve the reaction efficiency of the reaction between aluminum hydroxide and lactic acid; in addition, the sufficient amount of amorphous aluminum hydroxide can also improve the morphology of the generated aluminum lactate powder, and can improve the fluidity and dispersibility of the aluminum lactate powder, thereby accelerating the neutralization reaction. The reaction proceeds, thereby ultimately improving the reaction efficiency of the reaction between aluminum hydroxide and lactic acid; in addition, the lactic acid solution may also include a hydrophilic solvent, and the weight m3 of the hydrophilic solvent and the weight m2 of the amorphous aluminum hydroxide may satisfy the relationship: m3:m2=1:(0.12-0.59), so that the lactic acid solution has sufficient solvent, and the sufficient amount of solvent can effectively disperse the lactic acid solute of the lactic acid solution, and can improve the neutralization reaction between the lactic acid solute of the lactic acid solution and the amorphous aluminum hydroxide, so as to accelerate the progress of the neutralization reaction, thereby ultimately improving the reaction efficiency of the reaction between aluminum hydroxide and lactic acid.

[0058] The weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide can satisfy the relationship: m1:m2=1:0.24, 1:0.27, 1:0.30, 1:0.33, 1:0.36, 1:0.39, 1:0.42, 1:0.45, 1:0.48, 1:0.51, 1:0.54, 1:0.57, 1:0.60, 1:0.63, 1:0.66 or 1:0.67.

[0059] The weight m2 of the amorphous aluminum hydroxide can be 0.12, 0.15, 0.18, 0.21, 0.24, 0.27, 0.30, 0.33, 0.36, 0.39, 0.42, 0.45, 0.48, 0.51, 0.54, 0.57 or 0.59.

[0060] It should be noted that the purity of the lactic acid solute can be analytically pure (≥99%).

[0061] It should be noted that the hydrophilic solvent can be deionized water or ultrapure water.

[0062] In some optional embodiments, the temperature of the double hydrolysis reaction is ≤60°C, the time of the double hydrolysis reaction is 3h to 6h, and the pH of the double hydrolysis reaction is 12.0 to 13.5;

[0063] In these embodiments, the temperature of the double hydrolysis reaction can be ≤60°C, the pH of the double hydrolysis reaction can be 12.0-13.5, and the time of the double hydrolysis reaction can be 3h-6h, so as to promote the double hydrolysis reaction between the aluminate solution, the amorphous aluminum hydroxide seeds and the bicarbonate solution under strong alkaline conditions to obtain an amorphous aluminum hydroxide product with a complex surface morphology and more binding sites. The amorphous aluminum hydroxide can improve the reaction efficiency of the subsequent neutralization reaction.

[0064] The second preset stirring speed can be 600r / min, 610r / min, 620r / min, 630r / min, 640r / min, 650r / min, 660r / min, 670r / min, 680r / min, 690r / min, 700r / min, 750r / min, 800r / min, 850r / min, 900r / min, 950r / min or 1000r / min.

[0065] The temperature of the double hydrolysis reaction can be 60°C, 55°C, 50°C, 45°C, 40°C, 35°C, 30°C, 25°C or 20°C.

[0066] The pH of the double hydrolysis reaction can be 12.0, 12.1, 12.2, 12.3, 12.4, 12.5, 12.6, 12.7, 12.8, 12.9, 13.0, 13.1, 13.2, 13.3, 13.4 or 13.5.

[0067] The double hydrolysis reaction time can be 3.0 h, 3.5 h, 4.0 h, 4.5 h, 5.0 h, 5.5 h or 6.0 h.

[0068] In some optional embodiments, the drying temperature is 110° C. to 150° C., and the drying time is 50 min to 120 min; and / or

[0069] The temperature of the drying treatment is 60°C to 80°C, and the time of the drying treatment is 0.5h to 1.5h;

[0070] In these embodiments, the drying treatment temperature can be 110°C to 150°C, and the drying treatment time can be 50min to 120min, so that the aluminum lactate slurry generated between the lactic acid solute in the lactic acid solution and the amorphous aluminum hydroxide is fully dried to form an aluminum lactate powder product; in addition, the drying treatment temperature can be 60°C to 80°C, and the drying treatment time can be 0.5h to 1.5h. The liquid phase of the amorphous aluminum hydroxide wet material generated by the double hydrolysis reaction is fully removed by the drying treatment to obtain an amorphous aluminum hydroxide product with a complex surface morphology and more binding sites.

[0071] The drying temperature may be 110°C, 115°C, 120°C, 125°C, 130°C, 135°C, 140°C, 145°C or 150°C.

[0072] The drying time can be 50 min, 60 min, 70 min, 80 min, 90 min, 100 min, 110 min or 120 min.

[0073] The temperature of the drying process can be 60°C, 62°C, 64°C, 66°C, 68°C, 70°C, 72°C, 74°C, 76°C, 78°C or 80°C.

[0074] The drying time can be 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1.0h, 1.1h, 1.2h, 1.3h, 1.4h or 1.5h.

[0075] In some optional embodiments, the mass concentration of aluminum oxide in the aluminate-containing solution is 35 g / L to 79 g / L; and / or

[0076] The added amount m4 of the amorphous aluminum hydroxide seed crystals and the weight m5 of the aluminum oxide in the aluminate solution satisfy the relationship: m4:m5=(1-5):100.

[0077] In these embodiments, the mass concentration of aluminum oxide in the aluminate solution can be 35g / L to 79g / L, which enables the aluminate solution to have a sufficient amount of aluminum oxide. Under the regulation of amorphous aluminum hydroxide seeds, the sufficient amount of aluminum oxide will fully undergo a double hydrolysis reaction with the bicarbonate solution to obtain an amorphous aluminum hydroxide product with a complex surface morphology and more lactic acid binding sites. In addition, the added amount m4 of amorphous aluminum hydroxide seeds and the weight m5 of the alumina in the aluminate solution can satisfy the relationship: m4:m5=(1-5):100, which enables the double hydrolysis reaction to have a sufficient amount of amorphous aluminum hydroxide seeds. A sufficient amount of amorphous aluminum hydroxide seeds can accelerate the double hydrolysis reaction between the aluminate solution and the bicarbonate solution to obtain a large amount of amorphous aluminum hydroxide products.

[0078] The mass concentration of aluminum oxide in the aluminate solution can be 35g / L, 39g / L, 43g / L, 47g / L, 51g / L, 55g / L, 59g / L, 63g / L, 67g / L, 71g / L, 75g / L or 79g / L.

[0079] The added amount m4 of the amorphous aluminum hydroxide seed crystals and the weight m5 of the aluminum oxide in the aluminate solution can satisfy the relationship: m4:m5=1:100, 2:100, 3:100, 4:100 or 5:100.

[0080] In some optional embodiments, the mass concentration of bicarbonate in the bicarbonate solution is 36.75 g / L to 94.8 g / L; and / or

[0081] The bicarbonate solution comprises at least one of: sodium bicarbonate, potassium bicarbonate and ammonium bicarbonate;

[0082] In these embodiments, the mass concentration of bicarbonate in the bicarbonate solution can be 36.75 g / L to 94.8 g / L, so that the bicarbonate solution has a sufficient amount of bicarbonate, and under the regulation of amorphous aluminum hydroxide seeds, the sufficient amount of bicarbonate will fully undergo a double hydrolysis reaction with the aluminate solution to obtain an amorphous aluminum hydroxide product with a complex surface morphology and more binding sites; in addition, the bicarbonate solution can include: at least one of sodium bicarbonate, potassium bicarbonate and ammonium bicarbonate, so that the bicarbonate solution can have a sufficient amount of bicarbonate, and under the regulation of amorphous aluminum hydroxide seeds, the sufficient amount of bicarbonate will fully undergo a double hydrolysis reaction with the aluminate solution to obtain an amorphous aluminum hydroxide product with a complex surface morphology and more binding sites.

[0083] The mass concentration of bicarbonate in the bicarbonate solution can be 36.75 g / L, 37.00 g / L, 40.00 g / L, 43.00 g / L, 46.00 g / L, 49.00 g / L, 52.00 g / L, 55.00 g / L, 58.00 g / L, 61.00 g / L, 64.00 g / L, 67.00 g / L, 70.00 g / L, 73.00 g / L, 76.00 g / L, 79.00 g / L, 82.00 g / L, 85.00 g / L, 88.00 g / L, 91.00 g / L, 94.00 g / L or 94.8 g / L.

[0084] It should be noted that the alumina in the aluminate solution refers to the alumina form at the molecular structure level (AlO2 - ), rather than the presence of alumina solid (Al2O3) in the aluminate-containing solution.

[0085] Based on a general inventive concept, an embodiment of the present application provides an aluminum lactate powder, which is obtained by the preparation method.

[0086] The aluminum lactate powder is realized based on the above-mentioned preparation method. The specific steps of the preparation method can refer to the above-mentioned embodiment. Since the aluminum lactate powder adopts part or all of the technical solutions of the above-mentioned embodiments, it has at least all the beneficial effects brought by the technical solutions of the above-mentioned embodiments, which will not be described one by one here.

[0087] Based on a general inventive concept, an embodiment of the present application provides a binder, which includes the aluminum lactate powder.

[0088] The adhesive is realized based on the above-mentioned aluminum lactate powder. The specific composition of the aluminum lactate powder can refer to the above-mentioned embodiment. Since the adhesive adopts part or all of the technical solutions of the above-mentioned embodiment, it has at least all the beneficial effects brought by the technical solutions of the above-mentioned embodiment, which will not be repeated here one by one.

[0089] It should be noted that this adhesive is mainly based on aluminum lactate, which can replace existing organic adhesives for bonding refractory materials, plate-like objects and ceramic materials. Compared with traditional organic adhesives with defects such as high cost, environmental pollution, complicated operation process and strict usage methods, this adhesive has the advantages of low cost, short process, easy operation and green environmental protection.

[0090] Figure 2 A schematic flow chart of a method for preparing an adhesive provided in an embodiment of the present application is exemplarily shown;

[0091] Based on a general inventive concept, such as Figure 2As shown, the embodiment of the present application provides a method for preparing the adhesive, the method comprising:

[0092] S1. The aluminum powder, magnesium powder and the aluminum lactate powder are mixed to obtain a mixed powder;

[0093] S2. Grind the mixed powder to obtain aluminum lactate adhesive; wherein the weight m6 of the aluminum powder, the weight m7 of the magnesium powder and the weight m8 of the aluminum lactate powder satisfy the relationship: m6:m7:m8=(4~12):(10~18):(70~86).

[0094] The aluminum lactate powder is realized based on the above-mentioned preparation method. The specific steps of the preparation method can refer to the above-mentioned embodiment. Since the aluminum lactate powder adopts part or all of the technical solutions of the above-mentioned embodiments, it has at least all the beneficial effects brought by the technical solutions of the above-mentioned embodiments, which will not be described one by one here.

[0095] It should be noted that the mixing can be carried out in a three-dimensional mixer; and the grinding process can be carried out in a ball mill.

[0096] It should be noted that the weight m6 of aluminum powder, the weight m7 of magnesium powder and the weight m8 of aluminum lactate powder can satisfy the relationship: m6:m7:m8=(4-12):(10-18):(70-86). By adding aluminum powder and magnesium powder to aluminum lactate powder, the aluminum powder and magnesium powder can be used to fill the gaps in the aluminum lactate powder, thereby promoting uniform dispersion of the aluminum lactate powder, thereby improving the adhesion of the aluminum lactate powder and improving the adhesion ability of the adhesive.

[0097] It should be noted that the grinding media used for the grinding process may include alumina balls, and the weight m9 of the alumina balls and the weight m10 of the mixed powder may satisfy the relationship: m9:m10=(6-8):1, and the grinding process time may be 2.5h-5h. The alumina balls can effectively ball-mill the mixed powder to promote full and uniform dispersion of the aluminum powder, magnesium powder and aluminum lactate powder, thereby obtaining an aluminum lactate adhesive with uniform distribution and relatively fine particle size.

[0098] The weight m6 of the aluminum powder can be 4, 5, 6, 7, 8, 9, 10, 11 or 12; the weight m7 of the magnesium powder can be 10, 11, 12, 13, 14, 15, 16, 17 or 18; the weight m8 of the aluminum lactate powder can be 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85 or 86.

[0099] The weight m9 of the alumina ball can be 6, 7 or 8.

[0100] The grinding treatment time can be 2.5h, 3.0h, 3.5h, 4.0h, 4.5h or 5.0h.

[0101] It should be noted that the preparation method of aluminum lactate powder provided in the embodiment of the present application has the following advantages:

[0102] 1. High reaction efficiency and low cost: The loose structure and complex surface binding sites of amorphous aluminum hydroxide make its neutralization reaction with lactic acid solution faster and more complete, and the reaction temperature is low, which can reduce the energy consumption required for the preparation of aluminum lactate powder; in addition, the cost of amorphous aluminum hydroxide is lower than that of aluminum or other aluminum salts. The reaction of amorphous aluminum hydroxide with lactic acid can replace the reaction of metallic aluminum with lactic acid or the reaction of aluminum salt with lactic acid to prepare aluminum lactate powder, thereby greatly reducing the cost of raw materials and saving the production input cost of enterprises.

[0103] 2. Excellent product morphology: The generated aluminum lactate powder has a more regular morphology, which can avoid the agglomeration of aluminum lactate powder.

[0104] 3. High fluidity and dispersibility: The aluminum lactate powder with improved morphology has better fluidity and dispersibility, which is conducive to subsequent processing and application.

[0105] 4. Wide application: The aluminum lactate powder prepared by this preparation method can be mixed with magnesium powder and aluminum powder for ball milling to prepare aluminum lactate adhesive, so as to provide a new method for preparing adhesive. This method has the advantages of simple operation, short process and high preparation efficiency, and meets the requirements of green and low carbon.

[0106] The present application is further described below in conjunction with specific examples. The experimental methods in the following examples where specific conditions are not specified are usually measured in accordance with national standards / industry standards; if there are no corresponding national standards / industry standards, they are measured in accordance with common international standards, conventional conditions or conditions recommended by the manufacturer.

[0107] Example 1

[0108] like Figure 1 As shown, a method for preparing aluminum lactate powder comprises:

[0109] S101. A soluble salt containing bicarbonate is first stirred with a solvent to obtain a bicarbonate solution;

[0110] S102. Aluminate solution, amorphous aluminum hydroxide seed crystals and bicarbonate solution are subjected to a double hydrolysis reaction to obtain amorphous aluminum hydroxide wet material;

[0111] S103. Drying the wet amorphous aluminum hydroxide to obtain amorphous aluminum hydroxide;

[0112] S1. neutralizing the lactic acid solution and amorphous aluminum hydroxide to obtain an aluminum lactate slurry;

[0113] S2. Drying the aluminum lactate slurry to obtain an aluminum lactate powder product.

[0114] The temperature of the neutralization reaction is 30°C, and the time of the neutralization reaction is 45 min;

[0115] The neutralization reaction is carried out under the second stirring condition, and the second stirring speed is 450r / min.

[0116] The lactic acid solution includes a lactic acid solute and a hydrophilic solvent, and the weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m1:m2=270g:81g;

[0117] The weight m3 of the hydrophilic solvent and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m3:m2=81g:670g.

[0118] The temperature of the double hydrolysis reaction is 35°C, the time of the double hydrolysis reaction is 3h, and the pH of the double hydrolysis reaction is 12.5.

[0119] The drying temperature was 110°C and the drying time was 70 min.

[0120] The drying temperature was 70°C and the drying time was 1 h.

[0121] The first stirring speed is 600r / min;

[0122] The mass concentration of aluminum oxide in the aluminate solution is 35 g / L;

[0123] The added amount m4 of amorphous aluminum hydroxide seed crystals and the weight m5 of aluminum oxide in the aluminate solution satisfy the relationship: m4:m5=2:100.

[0124] The mass concentration of bicarbonate in the bicarbonate solution is 36.75 g / L;

[0125] Bicarbonate solution is a solution of sodium bicarbonate.

[0126] Aluminum lactate powder is obtained by the above preparation method.

[0127] A binder, the binder comprising the aluminum lactate powder of the second aspect

[0128] like Figure 2 As shown, a method for preparing an adhesive comprises:

[0129] S1. The aluminum powder, magnesium powder and aluminum lactate powder are mixed to obtain a mixed powder;

[0130] S2. The mixed powder is ground to obtain an aluminum lactate binder; wherein,

[0131] The weight m6 of aluminum powder, the weight m7 of magnesium powder and the weight m8 of aluminum lactate powder satisfy the relationship: m6:m7:m8=6:15:100;

[0132] The grinding media used in the grinding process include alumina balls, and the weight m9 of the alumina balls and the weight m10 of the mixed powder satisfy the relationship: m9:m10=6:1;

[0133] The grinding time is 2.5h.

[0134] Example 2

[0135] Based on the contents disclosed in Example 1, the following modifications are further made:

[0136] The temperature of the neutralization reaction is 30°C, and the time of the neutralization reaction is 45 min;

[0137] The weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m1:m2=125g:81g.

[0138] The weight m3 of the hydrophilic solvent and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m3:m2=215g:81g;

[0139] The temperature of the double hydrolysis reaction is 50°C, the time of the double hydrolysis reaction is 3 hours, and the pH of the double hydrolysis reaction is 12.0.

[0140] The drying temperature was 110°C and the drying time was 70 min.

[0141] The first stirring speed is 700r / min;

[0142] The mass concentration of aluminum oxide in the aluminate solution is 70 g / L;

[0143] The added amount m4 of amorphous aluminum hydroxide seed crystals and the weight m5 of aluminum oxide in the aluminate solution satisfy the relationship: m4:m5=3:100.

[0144] The mass concentration of bicarbonate in the bicarbonate solution is 36.75 g / L;

[0145] Bicarbonate solution is a solution of sodium bicarbonate.

[0146] The weight m6 of aluminum powder, the weight m7 of magnesium powder and the weight m8 of aluminum lactate powder satisfy the relationship: m6:m7:m8=15:20:100;

[0147] The grinding media used in the grinding process include alumina balls, and the weight m9 of the alumina balls and the weight m10 of the mixed powder satisfy the relationship: m9:m10=7:1.

[0148] Example 3

[0149] Based on the contents disclosed in Example 1, the following modifications are further made:

[0150] The temperature of the neutralization reaction is 30°C, and the time of the neutralization reaction is 30 min;

[0151] The second stirring speed is 550 r / min.

[0152] The lactic acid solution includes lactic acid solute, and the weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m1:m2=310g:81g.

[0153] The weight m3 of the hydrophilic solvent and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m3:m2=260g:81g.

[0154] The temperature of the double hydrolysis reaction is 35°C, the time of the double hydrolysis reaction is 3h, and the pH of the double hydrolysis reaction is 13.0.

[0155] The drying temperature was 125°C and the drying time was 45 min.

[0156] The drying temperature was 70°C and the drying time was 1 h.

[0157] The first stirring speed is 750r / min;

[0158] The mass concentration of aluminum oxide in the aluminate solution is 49 g / L;

[0159] The added amount m4 of amorphous aluminum hydroxide seed crystals and the weight m5 of aluminum oxide in the aluminate solution satisfy the relationship: m4:m5=4:100.

[0160] The mass concentration of bicarbonate in the bicarbonate solution is 72.38 / L;

[0161] The bicarbonate solution is a solution of potassium bicarbonate.

[0162] The weight m6 of aluminum powder, the weight m7 of magnesium powder and the weight m8 of aluminum lactate powder satisfy the relationship: m6:m7:m8=10:25:100;

[0163] The weight m9 of the alumina balls and the weight m10 of the mixed powder satisfy the relationship: m9:m10=6:1.

[0164] Example 4

[0165] Based on the contents disclosed in Example 1, the following modifications are further made:

[0166] The temperature of the neutralization reaction is 30°C, and the time of the neutralization reaction is 70 minutes.

[0167] The weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m1:m2=185g:81g;

[0168] The weight m3 of the hydrophilic solvent and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m3:m2=333g:81g.

[0169] The temperature of the double hydrolysis reaction is 58°C, the time of the double hydrolysis reaction is 3h, and the pH of the double hydrolysis reaction is 13.5.

[0170] The drying temperature was 110°C and the drying time was 70 min.

[0171] The first stirring speed is 600r / min;

[0172] The mass concentration of aluminum oxide in the aluminate solution is 75 g / L;

[0173] The added amount m4 of amorphous aluminum hydroxide seed crystals and the weight m5 of aluminum oxide in the aluminate solution satisfy the relationship: m4:m5=5:100.

[0174] The mass concentration of bicarbonate in the bicarbonate solution is 80.35 g / L;

[0175] The bicarbonate solution includes at least one of the following: sodium bicarbonate, potassium bicarbonate, and ammonium bicarbonate.

[0176] The weight m6 of aluminum powder, the weight m7 of magnesium powder and the weight m8 of aluminum lactate powder satisfy the relationship: m6:m7:m8=6:15:100;

[0177] The grinding media used in the grinding process include alumina balls, and the weight m9 of the alumina balls and the weight m10 of the mixed powder satisfy the relationship: m9:m10=8:1.

[0178] Comparative Example 1

[0179] Based on the contents disclosed in Example 3, the following modifications are further made:

[0180] No amorphous aluminum hydroxide is added, and conventional aluminum hydroxide is used directly.

[0181] Comparative Example 2

[0182] Based on the contents disclosed in Example 3, the following modifications are further made:

[0183] The preset stirring speed is less than 350 r / min, and the preset stirring speed is 300 r / min.

[0184] Comparative Example 3

[0185] Based on the contents disclosed in Example 3, the following modifications are further made:

[0186] The first stirring rotation speed is less than 600 r / min, and the first stirring rotation speed is 485 r / min.

[0187] Comparative Example 4

[0188] Based on the contents disclosed in Example 3, the following modifications are further made:

[0189] The pH of the double hydrolysis reaction is <12, and the pH of the double hydrolysis reaction is 10.5.

[0190] Comparative Example 5

[0191] Based on the contents disclosed in Example 3, the following modifications are further made:

[0192] The temperature of the neutralization reaction is <35°C, and the temperature of the neutralization reaction is 25°C.

[0193] Comparative Example 6

[0194] Based on the contents disclosed in Example 3, the following modifications are further made:

[0195] The temperature of the drying process is greater than 85°C, and the temperature of the drying process is 95°C.

[0196] Comparative Example 7

[0197] Based on the contents disclosed in Example 3, the following modifications are further made:

[0198] The temperature of the drying process is less than 85°C, and the temperature of the drying process is 75°C.

[0199] Comparative Example 8

[0200] Based on the contents disclosed in Example 3, the following modifications are further made:

[0201] The temperature of the drying process is >150°C, and the temperature of the drying process is 165°C.

[0202] Related experiments and effect data:

[0203] 1. The aluminum lactate powder obtained in each embodiment and comparative example was counted, and its phase structure and the time consumed by the neutralization reaction to prepare the aluminum lactate powder were detected. The results are shown in Table 1.

[0204] Table 1 Phase structure and preparation time of aluminum lactate powder in various embodiments and comparative examples

[0205]

[0206]

[0207] As can be seen from Table 1, the embodiment of the present application provides a method for preparing aluminum lactate powder, which uses amorphous aluminum hydroxide instead of traditional ordinary aluminum hydroxide, which can improve the reaction efficiency of the reaction between aluminum hydroxide and lactic acid, and shorten the time required for preparing aluminum lactate powder to within 0.5h, and the prepared aluminum lactate powder products are all high-purity aluminum lactate powder products.

[0208] 2. The adhesives obtained from each embodiment and comparative example were subjected to actual experiments.

[0209] Each binder was added to the alkaline refractory brick aggregate, and then the binder and the alkaline refractory brick aggregate were stirred for 10 minutes using a mixer, and then water was added and the first stirring was continued for 10 minutes, and finally pressed into shape to obtain an alkaline refractory brick blank; the obtained alkaline refractory brick blank was subjected to a flexural strength test under high temperature conditions according to the national standard GB / T3002-2017, and the results are shown in Table 2.

[0210] Table 2 Flexural strength of basic refractory bricks prepared by using binders in different embodiments and comparative examples

[0211]

[0212]

[0213] It can be seen from Table 2 that the binder provided in the embodiment of the present application, which is based on the above-mentioned aluminum lactate powder, can increase the flexural strength of the prepared basic refractory brick blanks under high temperature conditions of 1400°C to above 5.0 MPa.

[0214] In addition, it can be seen from Table 1 and Table 2 that according to the data of Example 3 and Comparative Example 3, under the condition that the second stirring speed is less than 600r / min, the preparation method cannot form amorphous aluminum hydroxide that meets the use requirements, and these amorphous aluminum hydroxides cannot completely react with lactic acid to form aluminum lactate powder products in the subsequent process, thereby affecting the use effect of the subsequent adhesive. According to the data of Example 3 and Comparative Example 4, it can be proved that when the preset pH is less than 12, the preparation method cannot form amorphous aluminum hydroxide, so that amorphous aluminum hydroxide cannot completely react with lactic acid to form aluminum lactate powder products, thereby affecting the use effect of the subsequent adhesive. In addition, according to the data of Example 3 and Comparative Example 5, when the neutralization reaction temperature is less than 35°C, the preparation method cannot form amorphous aluminum hydroxide that meets the use requirements, and the subsequent amorphous aluminum hydroxide cannot completely react with lactic acid to form aluminum lactate powder products, thereby affecting the use effect of the subsequent adhesive. In addition, according to the data of Example 3 and Comparative Example 6, when the drying temperature is greater than 85°C, the pore structure of the amorphous aluminum hydroxide generated by the double hydrolysis reaction may collapse, thereby reducing the reactivity of the amorphous aluminum hydroxide, and the subsequent neutralization reaction will not be able to completely react with lactic acid to generate an aluminum lactate powder product, thereby affecting the use effect of the subsequent binder. In addition, according to the data of Example 3 and Comparative Example 7, when the drying temperature is less than 60°C, the double hydrolysis reaction may not be able to generate amorphous aluminum hydroxide, and the subsequent neutralization reaction cannot completely react with lactic acid to generate an aluminum lactate powder product, thereby affecting the use effect of the subsequent binder. In addition, according to the data of Example 3 and Comparative Example 6, when the drying temperature is greater than 150°C, the excessively high drying temperature will cause the aluminum lactate powder to deteriorate or even decompose, thereby forming a mixture of aluminum lactate and lactic acid, thereby affecting the use effect of the subsequent binder.

[0215] In summary, the embodiment of the present application provides a method for preparing aluminum lactate powder, which uses amorphous aluminum hydroxide instead of traditional ordinary aluminum hydroxide, can improve the reaction efficiency of the reaction between aluminum hydroxide and lactic acid, and shorten the time required for preparing aluminum lactate powder to within 0.5 h, and the prepared aluminum lactate powder products are all high-purity aluminum lactate powder products.

[0216] In addition, an adhesive provided in an embodiment of the present application can replace traditional organic adhesives and be used for bonding refractory materials, plate-like objects and ceramic materials. The adhesive has the advantages of low cost, short process, easy operation and green environmental protection. The adhesive innovates the application fields and application scenarios of aluminum lactate powder and can improve the flexural strength of bonding materials under high temperature conditions.

[0217] The above description is only a specific implementation of the present application, so that those skilled in the art can understand or implement the present application. It will be apparent to those skilled in the art that various modifications to these embodiments are possible, and the general principles defined in the present application can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown in the present application, but will conform to the widest range consistent with the principles and novel features applied for by the present application.

Claims

1. A method for preparing aluminum lactate powder, the preparation method comprising: The lactic acid solution and the amorphous aluminum hydroxide are subjected to a neutralization reaction to obtain aluminum lactate slurry; Drying the aluminum lactate slurry to obtain an aluminum lactate powder product; Wherein, the preparation method of the amorphous aluminum hydroxide comprises: A soluble salt containing bicarbonate is first stirred with a solvent to obtain a bicarbonate solution; The aluminate solution, the amorphous aluminum hydroxide seed crystals and the bicarbonate solution are subjected to a double hydrolysis reaction to obtain an amorphous aluminum hydroxide wet material; The amorphous aluminum hydroxide wet material is dried to obtain amorphous aluminum hydroxide.

2. The preparation method according to claim 1, wherein the temperature of the neutralization reaction is 35°C to 60°C, and the time of the neutralization reaction is 30min to 75min; and / or The neutralization reaction is carried out under the second stirring condition, and the rotation speed of the second stirring is ≥350r / min.

3. The preparation method according to claim 1, wherein the lactic acid solution comprises a lactic acid solute and a hydrophilic solvent, and the weight m1 of the lactic acid solute and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m1:m2=1:(0.24-0.67); and / or The weight m3 of the hydrophilic solvent and the weight m2 of the amorphous aluminum hydroxide satisfy the relationship: m3:m2=1:(0.12-0.59).

4. The preparation method according to claim 1, wherein the temperature of the double hydrolysis reaction is ≤ 60°C, the time of the double hydrolysis reaction is 3h to 6h, and the pH of the double hydrolysis reaction is 12.0 to 13.

5.

5. The preparation method according to claim 1, wherein the drying temperature is 110°C to 150°C, and the drying time is 50min to 120min; and / or The temperature of the drying treatment is 60° C. to 80° C., and the time of the drying treatment is 0.5 h to 1.5 h.

6. The preparation method according to claim 1, wherein the mass concentration of aluminum oxide in the aluminate-containing solution is 35 g / L to 79 g / L; and / or The added amount m4 of the amorphous aluminum hydroxide seed crystals and the weight m5 of the aluminum oxide in the aluminate solution satisfy the relationship: m4:m5=(1-5):

100.

7. The preparation method according to claim 1, wherein the first stirring speed is ≥ 600 r / min; and / or The mass concentration of bicarbonate in the bicarbonate solution is 36.75 g / L to 94.8 g / L; and / or The bicarbonate solution includes at least one of the following: sodium bicarbonate, potassium bicarbonate and ammonium bicarbonate.

8. Aluminum lactate powder, wherein the aluminum lactate powder is obtained by the preparation method according to any one of claims 1 to 7.

9. A binder, comprising the aluminum lactate powder according to claim 7.

10. A method for preparing the adhesive according to claim 8, the method comprising: Mixing aluminum powder, magnesium powder and the aluminum lactate powder to obtain a mixed powder; The mixed powder is ground to obtain an aluminum lactate adhesive; wherein the weight m6 of the aluminum powder, the weight m7 of the magnesium powder and the weight m8 of the aluminum lactate powder satisfy the relationship: m6:m7:m8=(4-12):(10-18):(70-86).

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