CN117602967A - Purification method of ceramic material - Google Patents
Purification method of ceramic material Download PDFInfo
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- CN117602967A CN117602967A CN202311607586.3A CN202311607586A CN117602967A CN 117602967 A CN117602967 A CN 117602967A CN 202311607586 A CN202311607586 A CN 202311607586A CN 117602967 A CN117602967 A CN 117602967A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000000746 purification Methods 0.000 title claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 96
- 239000012535 impurity Substances 0.000 claims abstract description 82
- 239000002253 acid Substances 0.000 claims abstract description 74
- 150000007524 organic acids Chemical class 0.000 claims abstract description 25
- 239000003960 organic solvent Substances 0.000 claims abstract description 24
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 20
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
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- 238000005406 washing Methods 0.000 claims description 28
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 5
- 239000011707 mineral Substances 0.000 claims description 5
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
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- JVKRKMWZYMKVTQ-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C=NN(C=1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JVKRKMWZYMKVTQ-UHFFFAOYSA-N 0.000 description 2
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- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- KZEVSDGEBAJOTK-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[5-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CC=1OC(=NN=1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O KZEVSDGEBAJOTK-UHFFFAOYSA-N 0.000 description 1
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- SXAMGRAIZSSWIH-UHFFFAOYSA-N 2-[3-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,2,4-oxadiazol-5-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NOC(=N1)CC(=O)N1CC2=C(CC1)NN=N2 SXAMGRAIZSSWIH-UHFFFAOYSA-N 0.000 description 1
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 1
- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- CONKBQPVFMXDOV-QHCPKHFHSA-N 6-[(5S)-5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-2-oxo-1,3-oxazolidin-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C[C@H]1CN(C(O1)=O)C1=CC2=C(NC(O2)=O)C=C1 CONKBQPVFMXDOV-QHCPKHFHSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
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- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
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- 150000004767 nitrides Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
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- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/91—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics involving the removal of part of the materials of the treated articles, e.g. etching
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/53—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone involving the removal of at least part of the materials of the treated article, e.g. etching, drying of hardened concrete
- C04B41/5315—Cleaning compositions, e.g. for removing hardened cement from ceramic tiles
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Cleaning By Liquid Or Steam (AREA)
Abstract
The invention relates to the technical field of ceramic material purification, and provides a ceramic material purification method. The method comprises the following steps: step S1: the ceramic material to be purified is subjected to first contact with an organic solvent, and oily impurities are removed; step S2: the ceramic material treated in the step S1 is subjected to second contact with aqueous solution with the temperature of more than 70 ℃; step S3: thirdly contacting the ceramic material treated in the step S2 with a mixed acid solution, wherein the mixed acid solution comprises an organic acid solution and an inorganic acid solution; the content of the organic acid solution is smaller than the content of the inorganic acid solution. The purification method can rapidly remove impurities on the surface of the ceramic, and improve the purity and appearance quality of the ceramic; the method can not produce harmful waste gas, and accords with environmental protection regulations and standards; the method has good stability and reliability, is suitable for removing surface impurities of various ceramic products, and has relatively low cost.
Description
Technical Field
The invention relates to the technical field of ceramic material purification, in particular to a ceramic material purification method.
Background
Ceramics are an important material and have wide applications in numerous industrial and everyday life fields, such as in electronics, construction, medical equipment and porcelain manufacturing. However, the surface quality of ceramic articles is critical to their performance and aesthetics. In the process of ceramic manufacture, the surface is often contaminated with various impurities, such as oxides, metal ions, organic matters, etc., due to limitations of raw materials or production processes, and the impurities affect the mechanical properties, electrical properties and appearance quality of the ceramic product.
Therefore, the ceramic manufacturing industry is continually seeking efficient purification methods to remove impurities from the surface of these ceramic materials and to improve the quality and performance of ceramic articles. The acid cleaning method is a common purification method in the ceramic industry, but the traditional acid cleaning method has the problems of poor purification effect, poor environment protection and the like.
In view of the wide application of ceramics in various fields and the importance of the surface quality thereof, the development of an efficient and environment-friendly pickling purification method has important significance for improving the surface quality of ceramics.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a purification method of ceramic materials. According to the purification method, after the ceramic material is subjected to heat treatment, the mixed acid solution is adopted to carry out acid washing and impurity removal, so that impurities on the surface of the ceramic material can be removed rapidly, the purity and appearance quality of the ceramic material are improved, harmful waste gas can not be generated, and the method meets environmental protection regulations and standards.
In order to achieve the above object, a first aspect of the present invention provides a method for purifying a ceramic material, the method comprising the steps of:
step S1: the ceramic material to be purified is subjected to first contact with an organic solvent, and oily impurities are removed;
step S2: carrying out second contact on the ceramic material treated in the step S1 and an aqueous solution with the temperature of more than 60 ℃;
step S3: thirdly contacting the ceramic material treated in the step S2 with a mixed acid solution, wherein the mixed acid solution comprises an organic acid solution and an inorganic acid solution; the content of the organic acid solution in the mixed acid solution is smaller than the content of the inorganic acid solution.
The content of the organic acid solution is smaller than the content of the inorganic acid solution, which may be interpreted as that the volume ratio of the organic acid solution is smaller than the volume ratio of the inorganic acid solution in the mixed acid solution.
In the present invention, the impurities may include various types of impurities such as some grease, dirt, dust, etc. generated during cutting, grinding, polishing, transportation of the product, some Fe, cu, ni, co, al etc. metal elements present on the activated surface in the product having the metal elements on the surface thereof, etc. These impurities may affect the appearance and properties of the ceramic material.
The inventor of the present invention has studied and found that in order to improve the effect of acid washing to remove impurities in the prior art, an acid solution is generally directly heated, but the acid solution is easily volatilized after being heated, so that harmful gas is leaked, and the environment is polluted. In order to better improve the removal of impurities on the surface of the ceramic and reduce the influence of harmful gases on the environment, the invention creatively provides a method for improving the impurity molecules on the surface of the ceramic and the activity of the molecules on the surface of the ceramic after the ceramic is subjected to heat treatment, so that the impurities on the surface of the ceramic are easier to remove during acid washing, further the impurities on the surface of the ceramic can be removed rapidly, the purity and the appearance smoothness of the ceramic are improved, and the service performance of the ceramic is improved.
The invention also adopts the mixed acid solution containing the combination of the organic acid solution and the inorganic acid solution as the acid washing solution, and the organic acid and the inorganic acid play a synergistic effect, thereby improving the effect of removing impurities. The inorganic acid can promote dissolution and exposure of impurities due to its strong acidity, making it easier to remove. The organic acid can form a complex with part of impurities, so that solid precipitation is realized, and the impurities are effectively removed.
In addition, the content of the organic acid solution is smaller than that of the inorganic acid solution, the inorganic acid with a larger content ratio can enable impurities to be better exposed and dissolved in the mixed acid solution, and the organic acid can be combined with the impurities to effectively remove the impurities (for example, the organic acid and impurity metal ions are complexed to form solid-state precipitates to realize impurity removal). Inorganic acid has stronger acidity generally, and can generate larger acidity effect even if the concentration is lower; while organic acids are typically used at lower concentrations because they are relatively weak in acidity, but have chemical properties that have affinity for certain impurity metal ions and are capable of complexing with them to form solid precipitates for efficient removal. The mixed acid solution of the combination of the organic acid solution and the inorganic acid solution is used as the acid washing solution, so that the effect of removing impurities by acid washing is further improved, and the stability and the reliability of the method are also improved.
Step S1
The organic solvent for removing oily impurities on the surface of the ceramic material can be selected according to the properties of the ceramic material, or the organic solvent for removing the oil on the surface of the ceramic material is commonly used in the field.
In some embodiments, the organic solvent includes, but is not limited to, at least one of acetone, ethanol, ethyl acetate, or chloroform.
In some embodiments, the organic solvent is preferably acetone.
In some embodiments, the ceramic material to be purified is subjected to a first contact with an organic solvent, by which is meant that the surface of the ceramic material is contacted with the organic solvent and chemically reacted. The first contact is achieved in a number of ways, such as soaking the ceramic material in an organic solvent, rinsing the ceramic material with an organic solvent, etc.
In some embodiments, the ceramic material to be purified is immersed in an organic solvent (preferably fully immersed, with all surfaces of the ceramic material being in sufficient contact with the organic solvent), i.e., the first contact is by immersing. Wherein the conditions of the first contact include: the soaking time is 8-20min, the soaking temperature is 20-25 ℃ (when the room temperature meets the range, the temperature of the organic solvent is not required to be regulated, and the room temperature is kept).
The type of organic solvent is limited and preferred, and the manner and condition of the first contact can better remove oily impurities from the surface of the ceramic material.
Step S2
The ceramic material from which oily impurities are removed is contacted with a hot water solution (such as water or hydrogen peroxide solution) at a temperature above 70 ℃, so that the surface impurity molecules and the surface molecular activity of the ceramic material can be improved, and the impurities on the surface of the ceramic material can be removed more easily when entering an acid washing step. The pickling solution does not need to be heated, thereby reducing the leakage of harmful substance gas and playing a role in protecting the environment.
In some embodiments, the ceramic material is to be subjected to a second contact with an aqueous solution above 70 ℃, by "second contact" is meant that the surface of the ceramic material is in contact with the aqueous solution. The second contact is achieved in a number of ways, such as for example by immersing the ceramic material in an aqueous solution, rinsing the ceramic material with an aqueous solution, etc.
In some embodiments, the ceramic material is immersed in an aqueous solution above 70 ℃ (preferably fully immersed in the aqueous solution, with all surfaces of the ceramic material in sufficient contact with the aqueous solution), i.e., the second contact is by immersion. The soaking time is not particularly limited, and may be adjusted according to the kind of ceramic material and the impurity content.
In some embodiments, the aqueous solution is at a temperature of 70 to 90 ℃, such as 70 ℃, 72 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 85 ℃, 88 ℃, 90 ℃. The temperature of the water solution is optimized, so that impurity molecules on the surface of the ceramic material can be activated more effectively, and the effect of removing impurities by pickling is further improved.
In some embodiments, the time of the second contact (e.g., soaking time) is 20min-40min, e.g., 20min, 22min, 25min, 28min, 30min, 32min, 35min, 38min, 40min. The soaking time is optimized, so that the effects that pickling and impurity removal cannot be effectively achieved due to too short time can be avoided, and the waste of time and cost caused by too long time can be avoided.
Step S3
The ceramic material is pickled by adopting a mixed acid solution, and chemical reaction is mainly carried out by utilizing a mixed acid solution with a specific concentration ratio and impurity molecules difficult to remove on the surface of the ceramic material, so that impurities are removed, and the quality performance, appearance and surface smoothness of the ceramic material are improved.
The third contact, i.e. the operation mode of pickling, is not particularly limited, for example, the ceramic material can be rinsed by adopting a mixed acid solution, or the ceramic material can be soaked by adopting a mixed acid solution, preferably, the soaking mode can better promote the pickling impurity removal effect.
In some embodiments, the mixed acid solution comprises an organic acid solution and a mineral acid solution. The organic acid and the inorganic acid play a synergistic role, so that the effect of removing impurities is improved.
In some embodiments, the organic acid solution is present in an amount less than the inorganic acid solution. The inorganic acid with more content ratio can make the impurity better exposed and dissolved in the mixed acid solution, and the organic acid can be combined with the impurity to effectively remove the impurity, further improves the effect of acid washing to remove the impurity.
In some embodiments, the mixed acid solution has a concentration of 8% -15%, for example, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%. When the concentration of the mixed acid solution is in the range, the ceramic material can be prevented from being corroded by too high acid concentration, the effect of acid washing and impurity removal can be prevented from being influenced by too low concentration, and therefore the ceramic material can be protected, and the efficient acid washing and impurity removal effect can be realized.
In the purification method of the present invention, it is necessary to monitor the concentration of the pickling solution (mixed acid solution), and the pickling solution is tested periodically (10 to 20 days) to ensure that it is maintained within the above-defined range, so as to ensure that the pickling effectively removes impurities from the ceramic surface.
In some embodiments, the mineral acid solution includes, but is not limited to, at least one of nitric acid, hydrofluoric acid, sulfuric acid, carbonic acid, hydrochloric acid.
In some preferred embodiments, the mineral acid solution is a combination of nitric acid and hydrofluoric acid. Wherein the concentration of the nitric acid solution is 8-13%. The concentration of the hydrofluoric acid solution is 8-13%.
In some embodiments, the organic acid solution includes, but is not limited to, at least one of acetic acid, oxalic acid, or citric acid.
In some preferred embodiments, the organic acid solution is acetic acid. Wherein the concentration of the acetic acid solution is 8-13%.
In some embodiments, the mixed acid solution comprises nitric acid, hydrofluoric acid, and acetic acid.
Although the inorganic acid solution and the organic acid solution are more in variety, through a large number of experiments, the invention surprisingly discovers that the inorganic acid solution formed by combining nitric acid and hydrofluoric acid and the acetic acid organic acid solution are prepared into a mixed acid solution, and can remarkably and efficiently improve the effect of removing impurities on the surface of the ceramic material by pickling.
In some embodiments, the mixed acid solution has a volume ratio of nitric acid, hydrofluoric acid, acetic acid, and solvent of (5-10): (0.5-4): (1-8): (80-93), preferably (6-8): (1-2): (2-5): (80-90). Wherein, when the mixed acid solution is prepared according to the volume ratio, the concentration of the nitric acid solution is 8-13%, the concentration of the hydrofluoric acid solution is 8-13%, and the concentration of the acetic acid solution is 8-13%.
In some embodiments, the solvent in the mixed acid solution comprises water, preferably high purity water, distilled water, or the like, free of impurities.
In some embodiments, the mixed acid solution has a pH of 1 to 3. Besides limiting the concentration of the mixed acid solution, the invention further limits the pH value of the mixed acid solution in the above range, so that the acidity of the mixed acid solution can be kept within a certain range, thereby improving the stability and reliability of the purification method of the ceramic material.
In some embodiments, the third contact (acid wash) time is 8-20min, e.g., 8min, 10min, 12min, 15min, 18min, 20min. Preferably, the pickling time is 10-15min. The pickling time is limited to the above range, and further preferably the pickling time, the effect of pickling impurity removal can be improved better.
In some embodiments, the method further comprises a pre-rinse step prior to step S1. That is, before the ceramic material is used for removing oily impurities by using an organic solvent, the ceramic material needs to be pre-washed and primarily cleaned, so that impurities adhered to the surfaces of dust and the like which are easy to wash away are removed.
In some embodiments, the pre-flush comprises: and (3) washing the ceramic material to be purified by pure water, and then soaking in the pure water. For example: washing the ceramic material to be purified with pure water for 3-10min, and soaking in pure water for 8-20min. The ceramic material to be purified is washed and soaked by pure water, so that certain impurities (such as dust) which are easy to remove on the surface of the ceramic material can be effectively removed, the subsequent step sequence of removing oily impurities is facilitated, and the effect of removing the impurities is integrally improved.
In some embodiments, the method further comprises a first drying between step S1 and step S2. After the ceramic material is soaked in the organic solvent in the step S1, the surface is adhered with the organic solvent, and the ceramic material needs to be dried for the first time and then subjected to subsequent hot water treatment. The first drying mode is not particularly limited, and for example, inert gas may be used for drying, for example, a nitrogen gun may be used for drying until the surface is free from water stains.
In some embodiments, the method further comprises a second drying between step S2 and step S3. And S2, after the ceramic material is soaked in hot water, the surface is adhered with an aqueous solution, and acid liquor can be diluted by directly carrying out acid washing, so that the concentration of the acid liquor is reduced, the acid washing effect is affected, and the subsequent acid washing treatment is required after the second drying. In order to ensure that the ceramic surface is not marked by water when immersed in acid solution, and to remove some of the removable impurity molecules remaining on the surface by the hot water immersion.
The secondary drying mode is not particularly limited, and for example, inert gas drying, such as nitrogen gun drying, can be adopted until the surface is free from water stain, or clean cloth and the like can be directly used for wiping the ceramic material, or the ceramic material is wiped and dried firstly and then dried by nitrogen.
In some embodiments, after the ceramic material is treated in step S3, a subsequent rinsing step is also performed, for example with pure water, in order to ensure the removal of the water mark and the removal of impurities remaining on the surface after pickling.
In some embodiments, the ceramic material is inspected for products both before and after purification in order to confirm whether the impurities visually apparent on the product are ultimately removed by comparison with the final post-purification inspection measurements. The inspection and measurement is a quality control step, and the quality control step is used for comparing the input inspection at the beginning and carrying out high-precision quality detection on the surface of the product, so that the product is ensured to have the impurity purification function.
In some embodiments, the specific operation flow of the purification method of the ceramic material provided by the invention is referred as follows: product inspection, pure water flushing, organic solvent soaking, flushing and blow-drying, hot water soaking, scrubbing and blow-drying, mixed acid soaking, flushing and blow-drying, inspection and measurement.
In some embodiments, the method for purifying a ceramic material provided by the invention comprises the following steps:
(1) Product inspection: selecting a ceramic material to be purified, observing the ceramic material, and testing the impurity content;
(2) Washing with pure water: washing the ceramic material to be purified with pure water for 3-10min, and soaking in a pure water washing tank for 8-20min;
(3) Soaking in an organic solvent: soaking the ceramic material treated in the step (2) in an organic solvent for 8-20min at 20-25 ℃;
(4) Washing and blow-drying: drying the ceramic material treated in the step (3) by adopting a nitrogen gun until no water stain exists on the surface of the ceramic material;
(5) Soaking in hot water: soaking the ceramic material treated in the step (4) in hot water at 70-90 ℃ for 20-40min;
(6) Scrubbing and blow-drying: wiping the ceramic material treated in the step (5) and drying by adopting a nitrogen gun;
(7) Soaking in mixed acid: pickling the ceramic material treated in the step (6) by adopting a mixed acid solution for 8-20min; the concentration of the mixed acid solution is 8-15%, and the volume ratio of nitric acid, hydrofluoric acid, acetic acid and solvent in the mixed acid solution is (6-8): (1-2): (2-5): (80-90);
(8) Washing and blow-drying: taking out the ceramic material treated in the step (7) from the acid liquor, and flushing with pure water;
(9) Checking and measuring: observing the ceramic material obtained after the treatment in the step (8), and testing the impurity content.
In some specific embodiments, a pickling tank, a pure water cleaning tank and an air draft device are arranged, and are used for soaking ceramic products in the two tanks for cleaning, purifying and protecting the environment; the safety devices include gloves, goggles, masks, and other necessary safety devices to ensure the safety of the operator.
The purification method of the ceramic material provided by the invention can effectively solve the problems of impurities existing on the surfaces of ceramic substances such as silicate, aluminate, refractory metal oxide, metal nitride, boride and the like, and improve the quality of products and the surface smoothness.
The technical scheme adopted by the invention has the following beneficial effects:
(1) The purification method of the ceramic material provided by the invention has high efficiency, can rapidly remove impurities on the surface of the ceramic, and improves the purity and appearance quality of the ceramic, thereby improving the service performance of the ceramic.
(2) The purification method of the ceramic material provided by the invention is environment-friendly, and the acid washing process used can not produce harmful waste gas, thereby conforming to environmental regulations and standards.
(3) The purification method of the ceramic material provided by the invention has good stability and reliability, and is suitable for removing surface impurities of various ceramic products.
(4) The purification method of the ceramic material provided by the invention has the advantages of relatively low cost, simple steps, no need of expensive equipment, suitability for large-scale production and hopeful reduction of production cost.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein. Herein, unless otherwise specified, data ranges all include endpoints.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
Unless defined otherwise, all scientific and technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention relates.
The technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified. The invention is described in detail below in connection with specific embodiments, which are intended to be illustrative rather than limiting.
A batch of silicate ceramic material to be purified is prepared, the appearance grade is judged to be G5, the impurity content grade is judged to be L5, and a specific reference standard is shown in the following detection method. The above ceramic materials to be purified were purified according to the purification methods of the ceramic materials of the following examples and comparative examples, except that some process parameters were different,the specific differences are shown in Table 1。
The purifying method of the ceramic material comprises the following steps:
(1) Product inspection: selecting a ceramic material to be purified, observing the ceramic material, and testing the impurity content;
(2) Washing with pure water: washing the ceramic material to be purified by pure water for 5min, and then placing the ceramic material into a pure water washing tank for soaking for 10min;
(3) Soaking in an organic solvent: soaking the ceramic material treated in the step (2) in an organic solvent for 8-20min at normal temperature;
(4) Washing and blow-drying: drying the ceramic material treated in the step (3) by adopting a nitrogen gun until no water stain exists on the surface of the ceramic material;
(5) Soaking in hot water: soaking the ceramic material treated in the step (4) in hot water at 70-90 ℃ for 20-40min;
(6) Scrubbing and blow-drying: wiping the ceramic material treated in the step (5) and blow-drying the ceramic material by a nitrogen gun;
(7) Soaking in mixed acid: pickling the ceramic material treated in the step (6) by adopting a mixed acid solution for 8-20min; the concentration of the mixed acid solution is 8% -15%;
(8) Washing and blow-drying: taking out the ceramic material treated in the step (7) from the acid liquor, and flushing with pure water;
(9) Checking and measuring: observing the ceramic material obtained after the treatment in the step (8), and testing the impurity content.
TABLE 1
Example 8 group
With reference to example 1, the difference is that the type of ceramic material is different;
example 8-1: boride ceramic material replaces silicate ceramic material, the appearance grade is G5, and the impurity content grade is L5;
example 8-2: the aluminate ceramic material replaces silicate ceramic material, the appearance grade is G5, and the impurity content grade is L5.
The ceramic materials purified in the above examples and comparative examples were subjected to the relevant performance test, and the test methods are described below:
(1) Appearance quality
The ceramic materials purified in each of the examples and comparative examples were observed and classified according to the following criteria:
g1: the ceramic surface has no visible impurities and flaws, the surface quality is very high,
and G2: ceramic surfaces have some minor imperfections and impurities, but have no impact on the overall quality of the product G3: the defects and impurities on the surface of the ceramic exist to a certain extent, but the normal use of the product cannot be influenced;
and G4: the surface flaws and impurities of the ceramic are more, but the use of the product is not greatly influenced;
and G5: the ceramic surface has more flaws and impurities, and some of the flaws and impurities can even affect the use of the product.
The results after the test are recorded in table 2.
(2) Impurity content measurement
The ceramic materials purified in each example and comparative example were tested for metal impurity levels using GD-MS and classified as follows:
l1: the content of metal ions is less than or equal to 20ppm;
l2: the metal ion content is less than or equal to 20ppm and less than or equal to 50ppm;
l3: the metal ion content is less than or equal to 50ppm and less than or equal to 100ppm;
l4: the metal ion content is less than or equal to 999ppm and less than 100ppm
L5: the metal ion content was >999ppm.
The results after the test are recorded in table 2.
TABLE 2
| Appearance quality | Impurity content | |
| Example 1 | G1 | L1 |
| Example 1-1 | G2 | L2 |
| Examples 1 to 2 | G3 | L2 |
| Examples 1 to 3 | G4 | L3 |
| Example 2-1 | G2 | L2 |
| Example 2-2 | G3 | L3 |
| Examples 2 to 3 | G3 | L4 |
| Example 3-1 | G2 | L3 |
| Example 3-2 | G3 | L2 |
| Example 4-1 | G2 | L2 |
| Example 4-2 | G3 | L2 |
| Example 5-1 | G2 | L2 |
| Example 5-2 | G3 | L2 |
| Example 6-1 | G3 | L2 |
| Example 6-2 | G3 | L2 |
| Example 7-1 | G1 | L2 |
| Example 7-2 | G3 | L2 |
| Example 8-1 | G1 | L1 |
| Example 8-2 | G1 | L1 |
| Comparative examples 1 to 1 | G3 | L4 |
| Comparative examples 1 to 2 | G2 | L4 |
| Comparative examples 1 to 3 | G3 | L4 |
| Comparative example 2 | G3 | L3 |
| Comparative example 3 | G4 | L3 |
| Comparative example 4 | G4 | L3 |
As can be seen from the results in Table 2, in the purification method of the present invention, the ceramic material is subjected to heat treatment and then is subjected to acid washing and impurity removal by using a mixed acid solution, so that the impurities on the surface of the ceramic material can be rapidly removed, and the purity and the appearance quality of the ceramic material can be improved.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. Furthermore, it should be noted that the scope of the methods and apparatus in the embodiments of the present application is not limited to performing the functions in the order shown or discussed, but may also include performing the functions in a substantially simultaneous manner or in an opposite order depending on the functions involved, e.g., the described methods may be performed in an order different from that described, and various steps may also be added, omitted, or combined. Additionally, features described with reference to certain examples may be combined in other examples.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is to be construed as including any modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (10)
1. A method for purifying a ceramic material, the method comprising the steps of:
step S1: the ceramic material to be purified is subjected to first contact with an organic solvent, and oily impurities are removed;
step S2: the ceramic material treated in the step S1 is subjected to second contact with aqueous solution with the temperature of more than 70 ℃;
step S3: thirdly contacting the ceramic material treated in the step S2 with a mixed acid solution, wherein the mixed acid solution comprises an organic acid solution and an inorganic acid solution;
the content of the organic acid solution in the mixed acid solution is smaller than the content of the inorganic acid solution.
2. The purification method according to claim 1, wherein the concentration of the mixed acid solution is 8% -15%;
and/or the pH value of the mixed acid solution is 1-3.
3. The purification method according to claim 1, wherein the mineral acid solution comprises at least one of nitric acid, hydrofluoric acid, sulfuric acid, carbonic acid, hydrochloric acid;
preferably, the mineral acid solution is a combination of nitric acid and hydrofluoric acid.
4. The purification method of claim 1, wherein the organic acid solution comprises at least one of acetic acid, oxalic acid, or citric acid;
preferably, the organic acid solution is acetic acid.
5. The purification method according to any one of claims 1 to 4, wherein the mixed acid solution comprises nitric acid, hydrofluoric acid, and acetic acid;
preferably, in the mixed acid solution, the volume ratio of nitric acid, hydrofluoric acid, acetic acid and solvent is (5-10): (0.5-4): (1-8): (80-93).
6. The purification method according to any one of claims 1 to 4, wherein the organic solvent comprises at least one of acetone, ethanol, ethyl acetate, or chloroform; acetone is preferred.
7. The method according to any one of claims 1 to 4, wherein in the step S1, the first contact time is 8 to 20 minutes.
8. The purification method according to any one of claims 1 to 4, wherein in the step S2, the temperature of the aqueous solution is 70 to 90 ℃; and/or the second contact time is 20-40min;
and/or, in the step S3, the time of the third contact is 8-20min.
9. The purification method according to any one of claims 1 to 4, further comprising a pre-rinse step prior to step S1;
preferably, the pre-flush comprises: and (3) washing the ceramic material to be purified by pure water, and then soaking in the pure water.
10. The method according to any one of claims 1 to 4, wherein the method further comprises a first drying between step S1 and step S2,
and/or the method further comprises a second drying between step S2 and step S3.
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