CN109437268B - Method for improving activity of superfine and ultra-white aluminum hydroxide micro powder - Google Patents
Method for improving activity of superfine and ultra-white aluminum hydroxide micro powder Download PDFInfo
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- CN109437268B CN109437268B CN201811499935.3A CN201811499935A CN109437268B CN 109437268 B CN109437268 B CN 109437268B CN 201811499935 A CN201811499935 A CN 201811499935A CN 109437268 B CN109437268 B CN 109437268B
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Abstract
The invention relates to the technical field of improving the quality of aluminum hydroxide micro powder, in particular to a method for improving the activity of ultra-fine and ultra-white aluminum hydroxide micro powder, controlling the addition amount of the active seed crystal solution to decompose and separate out aluminum hydroxide micro powder slurry from the sodium aluminate solution, filtering to obtain filter cake, neutralizing with hot water to obtain mixed solution, adding penetrant and dispersant, stirring, adding small amount of active crystal seed, and at the same time, aminopropyl trimethoxy silane oligomer is added as a modifier, the addition amount is controlled, the activation index of the aluminum hydroxide micropowder is improved, and the sodium content in the prepared aluminum hydroxide micro powder is greatly reduced to be less than 0.073%, the quality of the aluminum hydroxide micro powder is greatly improved, the use amount of seed crystals is reduced, and the cost is reduced.
Description
Technical Field
The invention relates to the technical field of improving the quality of aluminum hydroxide micro powder, in particular to a method for improving the activity of ultra-fine and ultra-white aluminum hydroxide micro powder.
Background
The aluminum hydroxide micro powder is widely applied to the fields of flame retardance, filling and the like; at present, for the preparation of aluminum hydroxide micropowder, a sodium aluminate solution is decomposed to obtain an aluminum hydroxide slurry, the aluminum hydroxide slurry is separated by a filter, and the aluminum hydroxide slurry is obtained by twice reverse washing with hot water, for example, in patent No. 201610171923.2, a carbonated sodium aluminate solution is adopted, aluminum hydroxide seed crystals are obtained and added into the sodium aluminate solution, the aluminum hydroxide seed crystals are decomposed by temperature-changing seed decomposition to obtain decomposed slurry, iron is removed, depolymerization is carried out, water is removed, and the micropowder aluminum hydroxide is obtained by scattering and classification; and carrying out carbonation treatment within the temperature range of 60-75 ℃, after adding seed crystals for 4-10h, controlling the temperature to be 45-60 ℃ for decomposition, and heating to 55-70 ℃ before discharging decomposed slurry, so that the prepared micro powder product has stable quality, the ferric oxide is less than or equal to 0.008 percent, the sodium oxide is between 0.083-0.100 percent, and the whiteness is between 96.9-98.8 percent.
However, the aluminum hydroxide has a large polarity and is easily affected by hydrogen bonds, so that the particles are very easy to agglomerate, and the compatibility between the aluminum hydroxide and the organic polymer is poor, so that the aluminum hydroxide is dispersed and unevenly distributed in the use process, and the aluminum hydroxide particles with large particles can cause stress concentration of the composite material, so that the processing performance and the mechanical property of the composite material are affected when the aluminum hydroxide is applied to the composite material, and the application and the storage of the aluminum hydroxide micropowder are greatly affected. Therefore, the surface of the aluminum hydroxide micropowder needs to be modified to achieve the purpose of improving the activity of the aluminum hydroxide micropowder.
At present, the surface modification adopts dry modification and wet modification, but the dry modification has the defects of uneven coating, low coating rate, generation of a large amount of dust and pollution to the production environment, and the aluminum hydroxide micro powder obtained by the dry modification is exposed in the air, so that secondary treatment needs to be carried out on the aluminum hydroxide micro powder, otherwise, the activity of the aluminum hydroxide micro powder is extremely low. Therefore, the wet modification treatment completely solves a plurality of problems existing in dry modification and has good modification effect; however, the currently commonly used modifier is a silane coupling agent, and the common silane coupling agent is insoluble in water, so that an emulsifier needs to be added for emulsification in the wet modification process, and then the silane coupling agent is uniformly dispersed in water, so that the modification effect is enhanced.
In view of the above, the researchers have aimed at the technical defects, using N-2-aminoethyl-3-aminopropyltrimethoxysilane, methoxy-isopropanol, catalyst and water as raw materials to prepare aminopropyltrimethoxysilane oligomer as modifier; mixing, crystallizing and decomposing aluminum hydroxide micro powder and a sodium aluminate solution, performing filter pressing and cleaning to obtain an aluminum hydroxide micro powder filter cake, adding the aluminum hydroxide micro powder filter cake into a pulping tank to prepare aluminum hydroxide slurry, pumping the aluminum hydroxide slurry into a modification tank, adding a modifier for modification, and drying to obtain the aluminum hydroxide slurry; the using amount of the modifying solution is reduced, the cost is reduced, the activation index of the modified aluminum hydroxide micropowder can reach 93-96.6%, and the quality of the aluminum hydroxide micropowder is greatly improved. However, in the above-mentioned method, the amount of the modifier added is controlled to be in the range of 0.8 to 1.5% during the operation, so that the activating effect of the modified aluminum hydroxide fine powder is still not satisfactory, and according to the description of the prior art, an appropriate amount of the modifier added contributes to the improvement of the activation index, but when the amount of the modifier added is increased, the amount of the modifier remaining in the aluminum hydroxide fine powder is increased improperly, so that the purity of the obtained aluminum hydroxide fine powder is lowered.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for improving the activity of superfine and ultra-white aluminum hydroxide micropowder.
The method is realized by the following technical scheme:
the method for improving the activity of the superfine and ultra-white aluminum hydroxide micropowder comprises the following steps:
(1) mixing aluminum hydroxide powder and water according to equal mass ratio, grinding for 1.2-2.8h by using a cell mill to obtain an aluminum hydroxide solution with the particle size of 1.8-2.2 mu m and the concentration of 330-;
(2) adding 0.0004-0.0008 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; placing the mixed solution in a crystallization reactor, controlling the temperature to be 60-70 ℃, reacting for 3-5h, and filtering to obtain filtrate and filter cake; returning the filtrate to prepare a sodium aluminate solution;
(3) dissolving the filter cake in hot water of 80 ℃ to obtain a mixed solution; adding 0.008 times of penetrating agent and 0.0009 times of dispersing agent into the mixed solution, stirring at a stirring speed of 100r/min for 1-3h, adding 0.0001 times of active seed crystal solution and modifying agent, filtering after 3h, washing with hot water at 70 ℃, wherein the adding amount of the modifying agent accounts for 1.7-2.6% of the mass of the filter cake.
Preferably, the penetrant is a mixture of citric acid and tartaric acid.
Preferably, the penetrating agent is a mixture of citric acid and tartaric acid according to a mass ratio of 1: 3-4.
Preferably, the penetrating agent is a mixture of citric acid and tartaric acid according to a mass ratio of 1: 3.5.
Preferably, the modifier is aminopropyltrimethoxysilane oligomer.
Preferably, the dispersant is a nitric acid solution with the concentration of 1.3-1.7 mol/L.
Preferably, the dispersant is a nitric acid solution with the concentration of 1.5 mol/L.
Preferably, the addition amount of the modifier is 2.0 percent, 2.2 percent or 2.6 percent of the mass of the filter cake.
In the process of preparing the aluminum hydroxide micropowder, the addition of the active seed crystal solution is controlled, so that the sodium aluminate solution is decomposed to separate out aluminum hydroxide micropowder slurry, a filter cake after filtration is dissolved and dispersed in hot water to form a mixed solution, a penetrating agent and a dispersing agent are added and stirred, the active seed crystal after stirring is added in a small amount again, and meanwhile, aminopropyltrimethoxysilane oligomer is added as a modifier, the addition is controlled, so that the activation index of the aluminum hydroxide micropowder is improved, the sodium content in the prepared aluminum hydroxide micropowder is greatly reduced to reach below 0.073%, the quality of the aluminum hydroxide micropowder is greatly improved, the use amount of the seed crystal is reduced, and the cost is reduced.
Drawings
FIG. 1 is a relationship between the addition amount of a modifier and the activation index of aluminum hydroxide micropowder.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
Example 1
The method for improving the activity of the superfine and ultra-white aluminum hydroxide micropowder comprises the following steps:
(1) mixing aluminum hydroxide powder and water according to equal mass ratio, grinding for 1.2h by using a cell mill to obtain an aluminum hydroxide solution with the particle size of 1.8 mu m and the concentration of 330g/L, and taking the aluminum hydroxide solution as an active seed crystal solution;
(2) adding 0.0004 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; placing the mixed solution in a crystallization reactor, controlling the temperature to be 60 ℃, reacting for 3 hours, and filtering to obtain filtrate and filter cake; returning the filtrate to prepare a sodium aluminate solution;
(3) dissolving the filter cake in hot water of 80 ℃ to obtain a mixed solution; adding 0.008 times weight of mixture of citric acid and tartaric acid according to the mass ratio of 1:3 and 0.0009 times weight of nitric acid solution with the concentration of 1.3mol/L into the mixed solution, stirring at the stirring speed of 100r/min for 1h, adding 0.0001 times weight of active seed crystal solution and aminopropyltrimethoxysilane oligomer serving as modifiers, filtering after 3h, washing with hot water at 70 ℃, wherein the addition amount of the modifiers accounts for 1.7 percent of the mass of the filter cake.
Comparative example 1: in step (3) of example 1, after completion of stirring, it was directly filtered and washed to obtain a control 1.
Example 2
The method for improving the activity of the superfine and ultra-white aluminum hydroxide micropowder comprises the following steps:
(1) mixing aluminum hydroxide powder and water according to an equal mass ratio, grinding for 2.8 hours by using a cell mill to obtain an aluminum hydroxide solution with the particle size of 2.2 mu m and the concentration of 380g/L, and taking the aluminum hydroxide solution as an active seed crystal solution;
(2) adding 0.0008 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; placing the mixed solution in a crystallization reactor, controlling the temperature to be 70 ℃ for 5 hours of reaction, and filtering to obtain filtrate and filter cake; returning the filtrate to prepare a sodium aluminate solution;
(3) dissolving the filter cake in hot water of 80 ℃ to obtain a mixed solution; adding 0.008 times weight of mixture of citric acid and tartaric acid according to the mass ratio of 1:4 and 0.0009 times weight of nitric acid solution with the concentration of 1.7mol/L into the mixed solution, stirring at the stirring speed of 100r/min for 3h, adding 0.0001 times weight of active seed crystal solution and aminopropyltrimethoxysilane oligomer serving as modifiers, filtering after 3h, washing with hot water at 70 ℃, wherein the addition amount of the modifiers accounts for 2.6 percent of the mass of the filter cake.
Comparative example 2: in step (3) of example 2, after completion of stirring, it was directly filtered and washed to obtain control 2.
Example 3
The method for improving the activity of the superfine and ultra-white aluminum hydroxide micropowder comprises the following steps:
(1) mixing aluminum hydroxide powder and water according to equal mass ratio, grinding for 2.3h by using a cell mill to obtain an aluminum hydroxide solution with the particle size of 1.9 mu m and the concentration of 360g/L, and taking the aluminum hydroxide solution as an active seed crystal solution;
(2) adding 0.0007 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; placing the mixed solution in a crystallization reactor, controlling the temperature to be 65 ℃ for reaction for 4 hours, and filtering to obtain filtrate and filter cake; returning the filtrate to prepare a sodium aluminate solution;
(3) dissolving the filter cake in hot water of 80 ℃ to obtain a mixed solution; adding 0.008 times weight of mixture of citric acid and tartaric acid according to the mass ratio of 1:3.5 and 0.0009 times weight of nitric acid solution with the concentration of 1.5mol/L into the mixed solution, stirring at the stirring speed of 100r/min for 2h, adding 0.0001 times weight of active seed crystal solution and aminopropyltrimethoxysilane oligomer serving as modifiers, filtering after 3h, washing with hot water at 70 ℃, wherein the adding amount of the modifiers accounts for 2.2 percent of the mass of the filter cake.
Comparative example 3: in step (3) of example 3, after completion of stirring, it was directly filtered and washed to obtain a control 3.
Example 4
The method for improving the activity of the superfine and ultra-white aluminum hydroxide micropowder comprises the following steps:
(1) mixing aluminum hydroxide powder and water according to an equal mass ratio, grinding for 1.2h by using a cell mill to obtain an aluminum hydroxide solution with the particle size of 2.2 mu m and the concentration of 380g/L, and taking the aluminum hydroxide solution as an active seed crystal solution;
(2) adding 0.0004 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; placing the mixed solution in a crystallization reactor, controlling the temperature to be 60 ℃, reacting for 3 hours, and filtering to obtain filtrate and filter cake; returning the filtrate to prepare a sodium aluminate solution;
(3) dissolving the filter cake in hot water of 80 ℃ to obtain a mixed solution; adding 0.008 times weight of mixture of citric acid and tartaric acid according to the mass ratio of 1:4 and 0.0009 times weight of nitric acid solution with the concentration of 1.7mol/L into the mixed solution, stirring at the stirring speed of 100r/min for 2h, adding 0.0001 times weight of active seed crystal solution and aminopropyltrimethoxysilane oligomer serving as modifiers, filtering after 3h, washing with hot water at 70 ℃, wherein the addition amount of the modifiers accounts for 2.0 percent of the mass of the filter cake.
Comparative example 4: in step (3) of example 4, after completion of stirring, it was directly filtered and washed to obtain a control 4.
Example 5
The method for improving the activity of the superfine and ultra-white aluminum hydroxide micropowder comprises the following steps:
(1) mixing aluminum hydroxide powder and water according to equal mass ratio, grinding for 1.7h by using a cell mill to obtain an aluminum hydroxide solution with the particle size of 2.1 mu m and the concentration of 340g/L, and taking the aluminum hydroxide solution as an active seed crystal solution;
(2) adding 0.0005 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; placing the mixed solution in a crystallization reactor, controlling the temperature to be 70 ℃ for reaction for 4h, and filtering to obtain filtrate and filter cake; returning the filtrate to prepare a sodium aluminate solution;
(3) dissolving the filter cake in hot water of 80 ℃ to obtain a mixed solution; adding 0.008 times weight of mixture of citric acid and tartaric acid according to the mass ratio of 1:3 and 0.0009 times weight of nitric acid solution with the concentration of 1.6mol/L into the mixed solution, stirring at the stirring speed of 100r/min for 2.5h, adding 0.0001 times weight of active seed crystal solution and aminopropyltrimethoxysilane oligomer serving as modifiers, filtering after 3h, washing with hot water at 70 ℃, wherein the adding amount of the modifiers accounts for 2.3 percent of the mass of the filter cake.
Comparative example 5: in step (3) of example 5, after completion of stirring, it was directly filtered and washed to obtain control 5.
The sodium content of the aluminum hydroxide fine powder obtained in examples 1 to 5 and the control 1 to 5 was measured, and the results are shown in table 1 below:
TABLE 1
As can be seen from the data in Table 1, the treatment of adding the modifying step of the modifier and the addition of the active seed crystal solution are beneficial to improving the quality of the aluminum hydroxide micropowder and reducing the sodium content in the aluminum hydroxide micropowder.
In addition, during the research process, the researchers combined the micro-powder aluminum hydroxide prepared in examples 1-5 and the aluminum hydroxide micro-powder of reference 1-5, all dried in vacuum at 40 ℃ to constant weight, and weighed 5g, put into a graduated cylinder, added with 100mL distilled water, oscillated, stood, after the system is stabilized, removed the floating part on the water surface, dried, accurately weighed, and calculated the activation index of the aluminum hydroxide micro-powder according to the activity index of 100% × (floating mass/sample mass), the results are shown in table 2 below:
TABLE 2
As can be seen from the data in Table 2, the invention greatly improves the activation index of the prepared aluminum hydroxide micropowder and improves the quality of the aluminum hydroxide micropowder by adding the modifying agent and the active liquid crystal for modification.
In the course of the investigation, in order to understand the relationship between the amount of the modifier and the activation index of the fine aluminum hydroxide powder, the present inventors conducted the above-described working examples and based on example 1, for the relationship between the addition amount of the modifier and the activation index of the aluminum hydroxide micropowder, the researchers have continuously tried and tried, further, the relationship between the amount of the modifier added and the activation index of the fine aluminum hydroxide powder as shown in FIG. 1 was obtained, and as can be seen from FIG. 1, when the amount of the modifier added is less than 1.7%, the activation index of the aluminum hydroxide micro powder is unstable, when the addition amount of the modifier is more than 2.6 percent, the activation index of the aluminum hydroxide micro powder is greatly fluctuated, and the aluminum hydroxide powder has a downward trend, and when the addition amount of the modifier is between 1.7 and 2.6 percent, the activation index of the aluminum hydroxide powder is relatively stable, and the overall activation index is relatively high.
And as can be seen from the display in fig. 1, the activation index is better for the modifier added in an amount of 2.0% or 2.2% or 2.6% of the mass of the filter cake; based on the economic consideration, in the process of modification treatment, the modifier accounting for 2.0 percent of the mass of the filter cake is preferably added, so that the modification cost can be reduced, the activation index of the aluminum hydroxide micropowder is improved, the defect of low purity of the aluminum hydroxide micropowder caused by excessive addition can be effectively avoided, and the quality of the aluminum hydroxide micropowder is integrally improved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. A method for improving the activity of superfine ultra-white aluminum hydroxide micropowder comprises the following steps:
(1) mixing aluminum hydroxide powder and water according to equal mass ratio, grinding for 1.2-2.8h by using a cell mill to obtain an aluminum hydroxide solution with the particle size of 1.8-2.2 mu m and the concentration of 330-;
(2) adding 0.0004-0.0008 times of active seed crystal solution into the sodium aluminate solution to obtain a mixed solution; placing the mixed solution in a crystallization reactor, controlling the temperature to be 60-70 ℃, reacting for 3-5h, and filtering to obtain filtrate and filter cake; returning the filtrate to prepare a sodium aluminate solution;
(3) dissolving the filter cake in hot water of 80 ℃ to obtain a mixed solution; adding 0.008 times of penetrant and 0.0009 times of dispersant into the mixed solution, stirring at a stirring speed of 100r/min for 1-3h, adding 0.0001 times of active seed crystal solution and modifier, filtering after 3h, and washing with hot water at 70 ℃, wherein the addition amount of the modifier is 1.7-2.6% of the mass of the filter cake; the penetrating agent is a mixture of citric acid and tartaric acid according to a mass ratio of 1: 3-4; the modifier is aminopropyl trimethoxy silane oligomer; the dispersant is a nitric acid solution with the concentration of 1.3-1.7 mol/L.
2. The method for improving the activity of ultra-fine ultra-white aluminum hydroxide micropowder according to claim 1, wherein the penetrating agent is a mixture of citric acid and tartaric acid in a mass ratio of 1: 3.5.
3. The method for improving the activity of ultra-fine ultra-white aluminum hydroxide micropowder according to claim 1, wherein the dispersant is a nitric acid solution having a concentration of 1.5 mol/L.
4. The method of improving the activity of ultra-fine ultra-white aluminum hydroxide micropowder according to claim 1, wherein the modifier is added in an amount of 2.0% or 2.2% or 2.6% by mass of the filter cake.
5. The superfine ultra-white aluminum hydroxide micropowder obtained by the method for improving the activity of the superfine ultra-white aluminum hydroxide micropowder according to any one of claims 1 to 4.
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