CN109052442B - Production method of electronic grade high heat-resistant aluminum hydroxide - Google Patents
Production method of electronic grade high heat-resistant aluminum hydroxide Download PDFInfo
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- CN109052442B CN109052442B CN201811215489.9A CN201811215489A CN109052442B CN 109052442 B CN109052442 B CN 109052442B CN 201811215489 A CN201811215489 A CN 201811215489A CN 109052442 B CN109052442 B CN 109052442B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/46—Purification of aluminium oxide, aluminium hydroxide or aluminates
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a production method of electronic grade high heat-resistant aluminum hydroxide micropowder, which comprises the steps of removing impurities and purifying an aluminum hydroxide redissolution, adjusting solution molecules and controlling the decomposition speed, so that the aluminum hydroxide micropowder produced by the method has low impurity content, and the sodium oxide content reaches 0.08%; the granularity of the product is 1-6 mu m, and the granularity distribution is reasonable; good crystal growth, clear crystal boundary, perfect crystal appearance, sphere-like shape, high water loss temperature, and 1% water loss temperature of more than 245 ℃.
Description
Technical Field
The invention relates to a production method of aluminum hydroxide, in particular to a production method of electronic grade high heat-resistant aluminum hydroxide, belonging to the technical field of aluminum hydroxide preparation.
Background
In recent years, the technical level of domestic aluminum hydroxide is greatly improved, the granularity, the oil absorption rate and the whiteness of the product all reach a higher level, for example, the granularity of the product can reach 1-2 microns 5 years ago by using micro-powder aluminum hydroxide, but the granularity distribution is wider, the product is often accompanied by large particles, and the content of +325 is more than 0.1 percent; the oil absorption of the product is also above 40ml/100g, which has been solved by recent efforts. However, in the aluminum hydroxide process research in China, the dominant indexes such as particle size, oil absorption rate and whiteness are researched more, and the recessive indexes such as crystal morphology and application performance which affect the product performance are researched less.
Patent CN100391846C discloses a method for preparing high heat resistant aluminum hydroxide, which is to increase the decomposition temperature by surface modification method, although the decomposition temperature is increased to 262 ℃, the process is complicated, and the proportion of 262 ℃ decomposition is not described.
Patent ZL02153734.8 discloses a method for preparing an aluminum hydroxide flame retardant, which is characterized in that after sodium aluminate solution is purified, inorganic additives selected from calcium carbonate, aluminum silicate and phosphate are added for coating treatment; and adding 2-12% of surface modifier containing phosphorus silane or titanate for organic modification treatment, thereby greatly improving the heat resistance. But the process is complex and the cost is extremely high.
Therefore, in the prior art, research on a simple and economic process and a method for preparing electronic-grade aluminum hydroxide with purity and heat resistance reaching the requirements of the electronic-grade aluminum hydroxide is urgently needed, so that the requirements of the domestic copper-clad plate industry on the products are met, and the current industrial situation that the current industry mainly depends on import is reversed.
Disclosure of Invention
The invention provides a production method of electronic grade high heat-resistant aluminum hydroxide, which mainly researches the heat resistance, morphology and particle size distribution of the electronic grade aluminum hydroxide, and prepares an aluminum hydroxide product with good morphology development, good dispersibility and good thermal stability through the conditions of solution preparation, seed preparation, decomposition speed control and the like. The aluminum hydroxide produced by the method has low impurity content, and the content of sodium oxide reaches 0.08%; good crystal growth, clear crystal boundary, perfect crystal appearance, sphere-like shape, high water loss temperature, and 1% water loss temperature of more than 245 ℃.
The invention provides a production method of electronic grade high heat-resistant aluminum hydroxide, which comprises the following steps:
s1: adding liquid alkali into aluminum hydroxide for redissolving, adding water for diluting, adding an impurity removing agent for removing impurity elements, carrying out fine filtration to obtain a sodium aluminate solution, and adding water for diluting to obtain an electronic grade aluminum hydroxide decomposition stock solution;
s2: preparing seeds by a sand milling method;
s3: fine filtering the decomposition stock solution again, and then adding the seeds for decomposition;
s4: and separating mother liquor from the decomposed slurry, washing, and drying to obtain the aluminum hydroxide.
The electronic grade aluminum hydroxide has higher requirements on the physical properties of the powder and the content of impurities such as iron, sodium and the like of the product, so the preparation of the solution is important.
According to the production method of the aluminum hydroxide, the conventional aluminum hydroxide liquid adding alkali redissolution can be selected, the temperature is controlled to be 100-110 ℃ during redissolution, the alpha k of the solution is 1.4-2.2, and the concentration of sodium oxide is controlled to be 180-220 g/l.
According to the production method of the aluminum hydroxide, the dissolution liquid is diluted by adding water until the concentration of sodium oxide is 150-180 g/l.
Further, the sodium oxide is diluted until the concentration of the sodium oxide is preferably 160-170 g/l, and because the sodium aluminate solution is unstable when the alkali concentration is low, the loss of the aluminum oxide is increased when the impurity removal is carried out; however, the concentration is too high, which is not favorable for the impurity removal effect of the solution.
According to the production method of the aluminum hydroxide, the temperature is kept constant at 95 +/-5 ℃ in the impurity removal process, the addition amount of the impurity removal agent is 1-5 g/l, and the impurity removal time is controlled at 30-60 minutes.
Further, the impurity removing agent is activated carbon, silica gel, activated alumina or calcium oxide.
Furthermore, the addition amount of the impurity removing agent is preferably 2-4 g/l. The addition amount of the decoloring agent is crucial to the impurity removal and decoloring effect, the addition amount is small, the impurity removal effect is not obvious, and the whiteness of the product is low; the addition amount is too large, and the alumina loss is increased in the impurity removal process.
According to the production method of the aluminum hydroxide, the sodium aluminate solution obtained after fine filtration is diluted by adding water until the concentration of the alumina is 60-120 g/l, and then the electronic grade aluminum hydroxide decomposition stock solution is obtained.
According to the production method of the aluminum hydroxide, the granularity of the seeds is controlled to be 1-3 mu m when the seeds are prepared by a sand milling method; the solid content of the seeds is 200-300 g/l.
According to the production method of the aluminum hydroxide, the decomposed stock solution is subjected to fine filtration again, so that suspended matters in the solution are not higher than 0.02 g/l.
According to the production method of the aluminum hydroxide, seeds are added into the decomposition stock solution for decomposition, the alpha k of the decomposition stock solution is controlled to be 1.4-2.2, and the addition amount of the seeds is 0.2-2%.
Further, the decomposition raw liquid α k is preferably 1.6 to 1.9. The content of sodium oxide in the sample is increased when the alpha k of the decomposition stock solution is too low; if the decomposition raw liquid α k is too high, the yield is too low and the cost is high.
According to the production method of the aluminum hydroxide, the initial decomposition temperature is controlled to be 60-75 ℃, the final decomposition temperature is controlled to be 50-65 ℃, the temperature is slowly reduced from the initial temperature of 60-75 ℃ for decomposition, and the temperature reduction range is 0.5-1 ℃/h.
Further, the initial decomposition temperature is preferably 65-75 ℃, and the final decomposition temperature is preferably 55-65 ℃. The temperature of the sodium aluminate solution is related to the stability of the solution, and when the temperature is too low, the supersaturation degree of the solution is too high, the precipitation speed is too high, the crystal face development of crystals is influenced, the surface defects are increased, and the content of sodium oxide in the sample is increased; the temperature is too high, the supersaturation degree is too low, the precipitation speed is slow, the sample is easy to coarsen, and the yield is low.
According to the production method of the aluminum hydroxide, the decomposed slurry is washed after being separated from the mother liquor, and the temperature of washing water is more than or equal to 90 ℃ and the pH value is less than or equal to 7.5.
According to the production method of the aluminum hydroxide, the washing filter cake is dried, the drying temperature is controlled at 110 ℃, and the drying time is controlled at 8 hours, so that the aluminum hydroxide is obtained.
According to the production method, the aluminum hydroxide redissolution is subjected to impurity removal and purification, and the decomposition speed is controlled by adjusting solution molecules, so that the aluminum hydroxide produced by the method is low in impurity content, and the sodium oxide content reaches 0.08%; the granularity of the product is 1-6 mu m, and the granularity distribution is reasonable; good crystal growth, clear crystal boundary, perfect crystal appearance, sphere-like shape, high water loss temperature, and 1% water loss temperature of more than 245 ℃.
Drawings
FIG. 1 is an electron microscope morphology photograph of the aluminum hydroxide micropowder obtained by the production method of the present invention.
FIG. 2 is a thermogravimetric plot of the aluminum hydroxide micropowder obtained by the production method of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Example 1
Preparing an aluminum hydroxide redissolution, adding water to dilute the redissolution after dissolution until the concentration of sodium oxide is 150g/l, raising the temperature to 95 ℃, adding activated carbon to remove impurities, wherein the addition amount of an impurity removing agent is 1g/l, and the impurity removing time is controlled to be 40 minutes. Filtering, adding water for diluting until the concentration of alumina reaches 70g/l to obtain decomposition stock solution, adding 1000ml of decomposition stock solution into 12ml of seeds, controlling the initial decomposition temperature to be 75 ℃, the final decomposition temperature to be 60 ℃, the decomposition time to be 20 hours, washing and drying to obtain the aluminum hydroxide micropowder. The conditions and characteristics of the preparation of the redissolved solution used in example 1, the characteristics of the raw materials and the indices of the samples obtained are shown in tables 1, 2 and 3, respectively.
TABLE 1 redissolution preparation conditions and characteristics (same for other examples)
TABLE 2 raw material characteristics
TABLE 3 sample indices
Example 2
Preparing an aluminum hydroxide redissolution, adding water to dilute the redissolution after dissolution until the concentration of sodium oxide is 180g/l, raising the temperature to 90 ℃, adding silica gel to remove impurities, wherein the addition amount of an impurity removing agent is 5g/l, and the impurity removing time is controlled to be 60 minutes. Filtering, adding water for diluting until the concentration of alumina reaches 90g/l to obtain decomposition stock solution, adding 1000ml of decomposition stock solution into 12ml of seeds, controlling the initial decomposition temperature to be 75 ℃, the final decomposition temperature to be 60 ℃, the decomposition time to be 20 hours, washing and drying to obtain the aluminum hydroxide micropowder. The characteristics of the raw materials used in example 2 and the indices of the obtained samples are shown in tables 3 and 4, respectively.
TABLE 3 raw material characteristics
TABLE 4 sample indices
Example 3
Preparing an aluminum hydroxide redissolution, adding water to dilute the redissolution after dissolution until the concentration of sodium oxide is 160g/l, raising the temperature to 95 ℃, adding calcium oxide to remove impurities, wherein the addition amount of an impurity removing agent is 4g/l, and the impurity removing time is controlled to be 35 minutes. Filtering, adding water for diluting until the concentration of alumina reaches 110g/l to obtain decomposition stock solution, adding 1000ml of decomposition stock solution into 18ml of seeds, controlling the initial decomposition temperature at 70 ℃ and the final decomposition temperature at 60 ℃ for 25 hours, washing and drying to obtain the aluminum hydroxide micropowder. The characteristics of the raw materials used in example 3 and the indices of the obtained samples are shown in tables 5 and 6, respectively.
TABLE 5 raw Material characteristics
TABLE 6 sample indices
The granularity is analyzed by a Malvern 2000 granularity analyzer; the impurity content is analyzed by a chemical titration method; the specific surface is nitrogen adsorption method; the oil absorption rate is castor oil.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. A production method of electronic grade high heat-resistant aluminum hydroxide micropowder comprises the following steps:
s1: adding liquid alkali into aluminum hydroxide for redissolving, adding water for diluting, adding an impurity removing agent for removing impurity elements, carrying out fine filtration to obtain a sodium aluminate solution, and adding water for diluting to obtain an electronic grade aluminum hydroxide decomposition stock solution;
s2: preparing seeds by a sand milling method;
s3: fine filtering the decomposition stock solution again, and then adding the seeds for decomposition;
s4: separating mother liquor from the decomposed slurry, washing, and drying to obtain aluminum hydroxide micropowder;
controlling the temperature to be 100-110 ℃ during redissolution in S1, wherein the alpha k of the solution is 1.4-2.2, and the concentration of sodium oxide is controlled to be 180-220 g/L;
keeping the temperature constant at 95 +/-5 ℃ in the impurity removal process, wherein the adding amount of an impurity removal agent is 1-5 g/L, and the impurity removal time is controlled at 30-60 minutes;
the impurity removing agent is activated carbon, silica gel, activated alumina or calcium oxide;
controlling the seed granularity to be 1-3 mu m when preparing the seeds by a sand milling method; the solid content of the seeds is 200-300 g/L;
adding seeds into the decomposition stock solution for decomposition, wherein the alpha k of the decomposition stock solution is controlled to be 1.4-2.2, and the addition amount of the seeds is 0.2-2%;
the initial decomposition temperature is controlled to be 60-75 ℃, the final decomposition temperature is controlled to be 50-65 ℃, and the temperature reduction range is 0.5-1 ℃/h.
2. The method for producing aluminum hydroxide micropowder as claimed in claim 1, wherein the dilution is carried out by adding water to the dissolution liquid in S1 until the concentration of sodium oxide is 150 to 180 g/L.
3. The method for producing an aluminum hydroxide micropowder as claimed in claim 2, wherein the dilution is carried out until the concentration of sodium oxide is 160 to 170 g/L.
4. The method for producing aluminum hydroxide micropowder according to claim 3, wherein the amount of the impurity removing agent added is 2 to 4 g/L.
5. The method for producing the aluminum hydroxide micropowder as claimed in claim 1, wherein the sodium aluminate solution obtained after the fine filtration is diluted with water to an alumina concentration of 60 to 120g/L to obtain an electronic grade aluminum hydroxide decomposition stock solution.
6. A process for producing an aluminum hydroxide micropowder according to claim 5, characterized in that the decomposition raw liquid α k is controlled to 1.6 to 1.9.
7. A process for producing an aluminum hydroxide micropowder according to claim 6, wherein the initial decomposition temperature is 65 to 75 ℃ and the final decomposition temperature is 55 to 65 ℃.
8. The method for producing an aluminum hydroxide micropowder as claimed in claim 1, wherein the decomposed slurry is washed after separating a mother liquor, and the temperature of the washing water is not less than 90 ℃ and the pH is not more than 7.5.
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| CN1396116A (en) * | 2001-07-11 | 2003-02-12 | 住友化学工业株式会社 | Method for preparing aluminium hydroxide |
| CN101108740A (en) * | 2006-07-19 | 2008-01-23 | 中国科学院过程工程研究所 | Technique for processing bauxite to produce hydroted alumina with sodium hydroxide molten salt growth method |
| CN103221343A (en) * | 2010-04-16 | 2013-07-24 | 哈马诺材料有限公司 | Method for preparing high-urity aluminum hydroxide |
| CN106115755A (en) * | 2016-06-28 | 2016-11-16 | 上海滃泽科技有限公司 | A kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide |
| CN106186017A (en) * | 2016-07-26 | 2016-12-07 | 上海青平药业有限公司 | A kind of purification process of aluminium hydroxide powder |
| CN106915755A (en) * | 2015-12-27 | 2017-07-04 | 重庆任丙科技有限公司 | A kind of preparation method of high-purity alpha-alumina |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20180066456A (en) * | 2016-12-09 | 2018-06-19 | 주식회사 삼화양행 | Manufacturing method for high density bead of high purity alumina |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1396116A (en) * | 2001-07-11 | 2003-02-12 | 住友化学工业株式会社 | Method for preparing aluminium hydroxide |
| CN101108740A (en) * | 2006-07-19 | 2008-01-23 | 中国科学院过程工程研究所 | Technique for processing bauxite to produce hydroted alumina with sodium hydroxide molten salt growth method |
| CN103221343A (en) * | 2010-04-16 | 2013-07-24 | 哈马诺材料有限公司 | Method for preparing high-urity aluminum hydroxide |
| CN106915755A (en) * | 2015-12-27 | 2017-07-04 | 重庆任丙科技有限公司 | A kind of preparation method of high-purity alpha-alumina |
| CN106115755A (en) * | 2016-06-28 | 2016-11-16 | 上海滃泽科技有限公司 | A kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide |
| CN106186017A (en) * | 2016-07-26 | 2016-12-07 | 上海青平药业有限公司 | A kind of purification process of aluminium hydroxide powder |
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