CN108057681B - Cleaning method of aluminum oxide crucible of thermal weightlessness instrument - Google Patents
Cleaning method of aluminum oxide crucible of thermal weightlessness instrument Download PDFInfo
- Publication number
- CN108057681B CN108057681B CN201711033793.7A CN201711033793A CN108057681B CN 108057681 B CN108057681 B CN 108057681B CN 201711033793 A CN201711033793 A CN 201711033793A CN 108057681 B CN108057681 B CN 108057681B
- Authority
- CN
- China
- Prior art keywords
- instrument
- aluminum oxide
- thermal
- crucible
- weight loss
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004140 cleaning Methods 0.000 title claims abstract description 25
- 230000004580 weight loss Effects 0.000 claims abstract description 53
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 39
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001354 calcination Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000012360 testing method Methods 0.000 claims description 15
- -1 sulfate ester salt Chemical class 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 150000007942 carboxylates Chemical class 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- FVFJGQJXAWCHIE-UHFFFAOYSA-N [4-(bromomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CBr)C=C1 FVFJGQJXAWCHIE-UHFFFAOYSA-N 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- 229940057950 sodium laureth sulfate Drugs 0.000 claims description 2
- RUQIYMSRQQCKIK-UHFFFAOYSA-M sodium;2,3-di(propan-2-yl)naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S([O-])(=O)=O)=C(C(C)C)C(C(C)C)=CC2=C1 RUQIYMSRQQCKIK-UHFFFAOYSA-M 0.000 claims description 2
- SXHLENDCVBIJFO-UHFFFAOYSA-M sodium;2-[2-(2-dodecoxyethoxy)ethoxy]ethyl sulfate Chemical compound [Na+].CCCCCCCCCCCCOCCOCCOCCOS([O-])(=O)=O SXHLENDCVBIJFO-UHFFFAOYSA-M 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- 239000004711 α-olefin Substances 0.000 claims description 2
- PDGPUIMGYIBOLR-UHFFFAOYSA-N [Na].S(=O)(=O)(OC(CCCCCCCCCCC)=O)OCCN Chemical compound [Na].S(=O)(=O)(OC(CCCCCCCCCCC)=O)OCCN PDGPUIMGYIBOLR-UHFFFAOYSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims 1
- 229940051841 polyoxyethylene ether Drugs 0.000 claims 1
- 229920000056 polyoxyethylene ether Polymers 0.000 claims 1
- 150000003384 small molecules Chemical class 0.000 claims 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 5
- 239000003344 environmental pollutant Substances 0.000 description 5
- 231100000719 pollutant Toxicity 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000006864 oxidative decomposition reaction Methods 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
- B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
- B08B7/0085—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating by pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Detergent Compositions (AREA)
Abstract
The invention discloses a method for cleaning an alumina crucible of a thermal weightlessness instrument. The method comprises the following steps: the first step is as follows: putting an alumina crucible of a thermal weight loss instrument into an anionic surfactant aqueous solution for ultrasonic cleaning; the second step is that: placing the alumina crucible of the thermal weightlessness instrument after ultrasonic cleaning into a muffle furnace for calcination at the temperature of 600-900 ℃, wherein the calcination time is 30-120 minutes; the third step: putting the calcined alumina crucible of the thermal weightlessness instrument into water for ultrasonic cleaning; the fourth step: and (3) naturally airing the aluminum oxide crucible of the thermal weight loss instrument or drying the aluminum oxide crucible in an oven at 40-100 ℃. By the method, the aluminum oxide crucible of the thermal weightlessness instrument is cleaned, the recovery rate is high, and the method has the characteristics of convenience and rapidness in operation, safety, environmental friendliness and the like.
Description
Technical Field
The invention relates to a cleaning method, in particular to a cleaning method of an alumina crucible of a thermal weightlessness instrument.
Background
After the thermal weight loss test of chemicals is finished, residual substances in the alumina crucible are mainly carbon residue and inorganic powder, the volume of the crucible is small, the diameter of the crucible is only millimeter level, the crucible cannot be cleaned in a conventional mode, and if the crucible is directly abandoned without being cleaned, the cost is too high and resources are wasted.
The method generally used is a strong acid soaking method: usually, the insoluble matters are converted into soluble nitrates to be removed by soaking the mixture in nitric acid for a long time; then washing with water to remove soluble nitrate and residual inorganic powder; after drying, slowly heating to 800 ℃ in a high-temperature furnace for 6 hours to remove trace nitrate in the crucible; the cooled alumina crucible can be reused. However, this method is time consuming and requires the use of large amounts of strong acid, which is very corrosive, potentially dangerous to the operator and environmentally polluting.
Disclosure of Invention
The invention aims to provide a method for cleaning an alumina crucible of a thermal weightlessness instrument, which is safe, convenient and fast to operate and environment-friendly.
The invention is realized by the following technical scheme:
a cleaning method of an alumina crucible of a thermal weight loss instrument comprises the following steps:
the first step is as follows: putting an alumina crucible of a thermal weight loss instrument into an anionic surfactant aqueous solution, and carrying out ultrasonic cleaning in an ultrasonic cleaning instrument;
the second step is that: placing the alumina crucible of the thermal weightlessness instrument after ultrasonic cleaning into a muffle furnace for calcination at the temperature of 600-900 ℃, wherein the calcination time is 30-120 minutes;
the third step: putting the calcined alumina crucible of the thermal weightlessness instrument into water, and carrying out ultrasonic cleaning in an ultrasonic cleaning instrument;
the fourth step: and (3) naturally airing the aluminum oxide crucible of the thermal weight loss instrument or drying the aluminum oxide crucible in an oven at 40-100 ℃.
The aluminum oxide crucible of the thermal weight loss instrument is used for polluted aluminum oxide crucibles after the thermal weight loss test of chemicals, wherein the chemicals are at least one of organic micromolecules, inorganic substances, macromolecular compounds and plastics.
Wherein the anionic surfactant is at least one selected from carboxylate, sulfate ester salt, sulfonate and phosphate ester salt.
Wherein the carboxylate is at least one of sodium stearate, fatty acid potassium soap and ammonium oleate; the sulfate salt is at least one selected from sodium dodecyl sulfate, sodium laureth sulfate and sodium lauroylamidoethyl sulfate; the sulfonate is selected from at least one of sodium dodecyl benzene sulfonate, sodium petroleum sulfonate, sodium diisopropyl naphthalene sulfonate and sodium alpha-olefin sulfonate; the phosphate salt is at least one selected from sodium bis-decyl phosphate diester, disodium alkylphenol polyoxyethylene phosphate, and potassium fatty alcohol phosphate.
The concentration of the anionic surfactant aqueous solution is 1-5%.
Wherein, the ultrasonic cleaning temperature in the first step is 30-60 ℃, and the ultrasonic cleaning time is 3-30 minutes. Within this range, the ultrasonic cleaning effect is enhanced with an increase in temperature and with an increase in time.
In the method, a commercially available ultrasonic cleaning instrument can be used for ultrasonic cleaning, and the method can be as follows: VGT-900, Shanghai spectral laboratory science and technology Co., Ltd, 2500TH, VGT-1730QT, Guangdong Gute ultrasound industry Co., Ltd, Shanghai Qile electronics science and technology Co., Ltd.
Wherein the calcination temperature in the second step is 600-900 ℃, and the calcination time is 30-120 minutes. Wherein, when the calcining temperature is lower than 600 ℃, the calcining effect is not ideal and the cleaning effect is not good. After the calcining temperature is higher than 900 ℃, the probability of the alumina crucible damage of the thermal weight loss instrument is increased; similarly, when the calcination time is less than 30 minutes, the calcination effect is not satisfactory, and the cleaning effect is not good. And the calcination time is longer than 120 minutes, and the damage probability of the alumina crucible of the thermal weight loss instrument is increased.
According to the method, the muffle furnace can be a commercially available muffle furnace, and the highest temperature of the muffle furnace can meet the calcination requirement only when the highest temperature reaches over 600 ℃. Can be as follows: tonic electric furnace equipment Co., Ltd in Shanghai TCXC-1200, comet SX2-4-12, Yuhong photoelectricity YH-621A.
Wherein, the aluminum oxide crucible of the thermal weightlessness instrument is directly provided with water for the second step of calcination after being cleaned by ultrasonic waves in the first step. The calcination with water is carried out because at high temperature, the water promotes the oxidative decomposition of the residual carbon, so that the calcination time and temperature can be reduced, and the damage rate of the alumina crucible of the thermal weight loss instrument caused by calcination is reduced.
After the second step of calcination is completed, the temperature of the alumina crucible of the thermal weight loss instrument is reduced to 20-40 ℃, and then the alumina crucible is taken out.
The ultrasonic cleaning temperature in the third step is 30-60 ℃, and the ultrasonic cleaning time is 3-30 min.
The invention has the following beneficial effects:
the method comprises the steps of dispersing and taking out inorganic powder and partial residual carbon in an aluminum oxide crucible of a thermal weight loss instrument by utilizing ultrasonic vibration and an anionic surfactant, promoting oxidative decomposition of the residual carbon by utilizing water in the aluminum oxide crucible of the thermal weight loss instrument and high temperature of a muffle furnace, cleaning residual pollutants in the aluminum oxide crucible of the thermal weight loss instrument by utilizing ultrasonic vibration, and drying to obtain the clean aluminum oxide crucible of the thermal weight loss instrument which can be recycled. The cleaning method is convenient and fast to operate, the anionic surfactant which is safe to use replaces substances with strong oxidizing property and corrosivity such as common strong acid, the safety is improved, the cleaning time is shortened, the crucible recovery rate is high, and the cleaning effect is obvious.
Drawings
FIG. 1: comparative example 1 thermal weight loss curve of cleaned thermal weight loss instrument alumina crucible
FIG. 2: thermal weight loss curve of alumina crucible of new thermal weight loss instrument
FIG. 3: example 1 thermal weightlessness curve of cleaned thermal weightlessness instrument alumina crucible
FIG. 4: example 2 thermal weight loss curve of cleaned thermal weight loss instrument alumina crucible
FIG. 5: example 3 thermogravimetric curve of cleaned aluminum oxide crucible of thermogravimetric analyzer
Detailed Description
The present invention is further illustrated by the following specific examples, which are, however, not intended to limit the scope of the invention.
The raw materials used in the examples of the present invention were all commercially available.
The cleaning effect testing method comprises the following steps:
thermogravimetric analysis: placing the cleaned aluminum oxide crucible of the thermal weightlessness instrument into a thermal weightlessness instrument (relaxation-resistant model: TG209F3), and programming a temperature-raising program on an online software 'TG 209F3 on Usc 1': the temperature range is room temperature-testing temperature 750 ℃, the heating rate is 20K/min, and then the thermal weightlessness instrument carries out heating test according to the set heating program to obtain a thermal weightlessness curve; and then performing thermogravimetric analysis processing by using 'protein analysis' to obtain crucible mass change data at the end of the test.
Comparative example 1:
and (3) soaking the polluted aluminum oxide crucible of the thermal weight loss instrument after the thermal weight loss test of the polypropylene composition is finished in 98% concentrated sulfuric acid for 24h, washing with clear water, airing, placing in a muffle furnace, heating to 900 ℃, calcining for 30min, cooling, washing with water, and drying in an oven at 80 ℃ to obtain the cleaned aluminum oxide crucible of the thermal weight loss instrument. The cleaned aluminum oxide crucible of the thermal weightlessness instrument is subjected to a thermal weightlessness experiment to obtain the attached figure 1.
Example 1:
placing the alumina crucible of the polluted thermal weight loss instrument after the thermal weight loss test of the polypropylene composition is finished into the sodium dodecyl benzene sulfonate aqueous solution containing 1 percent of sodium dodecyl benzene sulfonate for ultrasonic cleaning for 10 minutes, wherein the ultrasonic cleaning temperature is 45 ℃; putting the alumina crucible of the thermal weight loss instrument with water after ultrasonic cleaning into a muffle furnace, heating to 900 ℃ and calcining for 30 min; after calcination, cooling to 30 ℃, and then putting the aluminum oxide crucible of the thermal weight loss instrument into water for ultrasonic cleaning for 10min at the ultrasonic cleaning temperature of 45 ℃; and naturally drying to obtain the aluminum oxide crucible of the thermal weight loss instrument with no pollutants on the surface. The cleaned aluminum oxide crucible of the thermal weightlessness instrument is subjected to a thermal weightlessness experiment to obtain the attached figure 3.
Example 2:
putting the polluted aluminum oxide crucible of the thermal weightlessness instrument after completing the sun-proof bright red BBN thermal weightlessness test into an aqueous solution containing 5 percent of lauryl sodium sulfate for ultrasonic cleaning for 3 minutes, wherein the ultrasonic cleaning temperature is 60 ℃; putting the alumina crucible of the thermal weight loss instrument with water after ultrasonic cleaning into a muffle furnace, heating to 600 ℃ and calcining for 120 minutes; after calcination, cooling to 30 ℃, and then putting the aluminum oxide crucible of the thermal weight loss instrument into water for ultrasonic cleaning for 3 minutes at the ultrasonic cleaning temperature of 60 ℃; and then placing the crucible in an oven at 80 ℃ for drying to obtain the aluminum oxide crucible of the thermal weight loss instrument with no pollutants on the surface. The cleaned aluminum oxide crucible of the thermal weightlessness instrument is subjected to a thermal weightlessness experiment to obtain the attached figure 4.
Example 3:
placing the aluminum oxide crucible of the thermal weight loss instrument polluted after the thermal weight loss test of the calcium carbonate powder is finished into an aqueous solution containing 3 percent of sodium stearate anionic surfactant for ultrasonic cleaning for 30 minutes at the ultrasonic cleaning temperature of 30 ℃; putting the alumina crucible of the thermal weight loss instrument with water after ultrasonic cleaning into a muffle furnace, heating to 800 ℃, and calcining for 60 min; after calcination is finished, cooling to 30 ℃, and then putting the aluminum oxide crucible of the thermal weight loss instrument into water for ultrasonic cleaning for 30 minutes at the ultrasonic cleaning temperature of 30 ℃; and then placing the crucible in a drying oven at 100 ℃ for drying and then cooling to obtain the thermal weightlessness instrument alumina crucible without pollutants on the surface. The cleaned aluminum oxide crucible of the thermal weightlessness instrument is subjected to a thermal weightlessness experiment to obtain the attached figure 5.
Table 1: performance test result of cleaned aluminum oxide crucible of thermal weightlessness instrument
The new aluminum oxide crucible of the heat loss instrument has the mass increased by 0.03mg after the thermal weight loss test, which is probably caused by indoor airflow; comparative example 1 the weight of the aluminum oxide crucible of the thermal weight loss instrument cleaned by the traditional acid cleaning method is reduced by 0.07mg after the thermal weight loss test, which shows that pollutants are remained in the aluminum oxide crucible of the thermal weight loss instrument cleaned by the method; the mass of the cleaned aluminum oxide crucibles of the thermal weight loss instruments of examples 1 to 3 respectively increased after the thermal weight loss test is close to the mass of the aluminum oxide crucibles of the new thermal weight loss instruments during the thermal weight loss test. Therefore, the method for cleaning the aluminum oxide crucible of the thermal weight loss instrument has good cleaning effect.
Claims (8)
1. A cleaning method of an alumina crucible of a thermal weightlessness instrument is characterized by comprising the following steps:
the first step is as follows: putting an alumina crucible of a thermal weight loss instrument into an anionic surfactant aqueous solution, and carrying out ultrasonic cleaning in an ultrasonic cleaning instrument;
the second step is that: putting the alumina crucible of the thermal weightlessness instrument after ultrasonic cleaning with water into a muffle furnace for calcination at the temperature of 600-900 ℃, wherein the calcination time is 30-120 minutes;
the third step: putting the calcined alumina crucible of the thermal weightlessness instrument into water, and carrying out ultrasonic cleaning in an ultrasonic cleaning instrument;
the fourth step: naturally airing the aluminum oxide crucible of the thermal weight loss instrument or drying the aluminum oxide crucible in an oven at 40-100 ℃;
the aluminum oxide crucible of the thermal weightlessness instrument is used for polluted aluminum oxide crucible of the thermal weightlessness instrument after the thermal weightlessness test of chemicals.
2. The method for cleaning an aluminum oxide crucible of a thermogravimetric analyzer according to claim 1, wherein the chemical is at least one of organic small molecules, inorganic substances and high molecular compounds.
3. The method for cleaning an aluminum oxide crucible of a thermogravimetric analyzer according to claim 1 or 2, wherein the anionic surfactant is at least one selected from the group consisting of carboxylate, sulfate ester salt, sulfonate and phosphate ester salt.
4. The method for cleaning an aluminum oxide crucible of a thermogravimetric analyzer according to claim 3, wherein the carboxylate is at least one selected from the group consisting of sodium stearate, potassium fatty acid soap, and ammonium oleate; the sulfate salt is at least one selected from sodium dodecyl sulfate, sodium laureth sulfate and sodium lauroyl aminoethyl sulfate; the sulfonate is selected from at least one of sodium dodecyl benzene sulfonate, sodium petroleum sulfonate, sodium diisopropyl naphthalene sulfonate and alpha-olefin sodium sulfonate; the phosphate salt is at least one selected from di-decyl phosphate diester sodium salt, alkylphenol polyoxyethylene ether phosphate disodium and fatty alcohol phosphate potassium salt.
5. The method for cleaning the aluminum oxide crucible of the thermogravimetric analyzer according to claim 1 or 2, wherein the concentration of the anionic surfactant aqueous solution is 1% -5%.
6. The method for cleaning the aluminum oxide crucible of the thermal weight loss instrument according to claim 1 or 2, wherein the ultrasonic cleaning temperature in the first step is 30-60 ℃; the ultrasonic cleaning time in the first step is 3-30 minutes.
7. The method for cleaning the aluminum oxide crucible of the thermal weight loss instrument according to claim 1 or 2, wherein the aluminum oxide crucible of the thermal weight loss instrument is taken out after the second step of calcination is completed and the temperature of the aluminum oxide crucible of the thermal weight loss instrument is reduced to 20-40 ℃.
8. The method for cleaning the aluminum oxide crucible of the thermal weight loss instrument according to claim 1 or 2, wherein the ultrasonic cleaning temperature in the third step is 30-60 ℃; the ultrasonic cleaning time in the third step is 3-30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711033793.7A CN108057681B (en) | 2017-10-30 | 2017-10-30 | Cleaning method of aluminum oxide crucible of thermal weightlessness instrument |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711033793.7A CN108057681B (en) | 2017-10-30 | 2017-10-30 | Cleaning method of aluminum oxide crucible of thermal weightlessness instrument |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108057681A CN108057681A (en) | 2018-05-22 |
| CN108057681B true CN108057681B (en) | 2020-10-23 |
Family
ID=62137987
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711033793.7A Active CN108057681B (en) | 2017-10-30 | 2017-10-30 | Cleaning method of aluminum oxide crucible of thermal weightlessness instrument |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108057681B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111482423A (en) * | 2020-04-08 | 2020-08-04 | 四川富乐德科技发展有限公司 | Cleaning regeneration method of titanium crucible |
| CN114130753A (en) * | 2021-11-24 | 2022-03-04 | 枣庄睿诺电子科技有限公司 | Process method for removing organic material residues in crucible |
| CN114472383A (en) * | 2022-01-26 | 2022-05-13 | 斯坦德检测集团股份有限公司 | Cleaning method of liner tube for pyrolysis gas chromatograph-mass spectrometer |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51125610A (en) * | 1975-04-25 | 1976-11-02 | Takemoto Oil & Fat Co Ltd | A mold-sash composition for cast-iron crvcibles for melting of metals |
| JP3552401B2 (en) * | 1996-03-22 | 2004-08-11 | 信越半導体株式会社 | Crucible cleaning method |
| CN1250347C (en) * | 2003-01-13 | 2006-04-12 | 中国科学院长春光学精密机械与物理研究所 | Chemical washing method of boron nitride crucible |
| CN103102183A (en) * | 2012-11-13 | 2013-05-15 | 三达奥克化学股份有限公司 | Cleaning agent for removing ferrocolumbium, copper and silicon sintering scale layer on inner wall of silicon carbide crucible as well as preparation method thereof |
| CN103424332A (en) * | 2013-09-02 | 2013-12-04 | 南京大学 | Method for measuring platinum carrying capacity of CCM and MEA of fuel cell |
-
2017
- 2017-10-30 CN CN201711033793.7A patent/CN108057681B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN108057681A (en) | 2018-05-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108057681B (en) | Cleaning method of aluminum oxide crucible of thermal weightlessness instrument | |
| CN105603409A (en) | Normal-temperature alkaline chromium-free passivation solution and passivation method for aluminum alloy | |
| CN105238488B (en) | A kind of dealkalization method of coal | |
| CN106045398A (en) | Method for preparing cracking-resistant low-shrinking cement mortar with modified coconut fibers | |
| CN104030344A (en) | Comprehensive treatment method for titanium tetrachloride dust collecting residue | |
| CN107188506A (en) | A kind of electrolytic manganese slag brick and its preparation technology | |
| Chen et al. | Leaching characteristics and kinetics of the metal impurities present in rice husk during pretreatment for the production of nanosilica particles | |
| CN103028581B (en) | Handling method of sand core crucible used for detecting insoluble quinoline | |
| CN106237655A (en) | A kind of preparation method of super-hydrophobic micro-nano zinc oxide copper mesh | |
| CN104232901A (en) | Method for casting aluminum part from recovered scrap aluminum cuttings | |
| CN102183392B (en) | Optimum digestion method in measuring heavy metals in waste rubber granules | |
| CN106092708B (en) | Corrosion display method for 300M steel grain size | |
| CN107937156A (en) | Efficient multienzyme cleaning agent of medical instrument and preparation method thereof | |
| CN102826513A (en) | Production process of hydrofluoric acid | |
| CN112649275A (en) | Microwave digestion solution and digestion method for HF-free automobile exhaust catalyst | |
| CN109437812A (en) | A kind of thermal insulation coatings and preparation method thereof | |
| CN105784452B (en) | Method for extracting and separating carbon black from vulcanized rubber | |
| CN112540104B (en) | Concrete matrix corrosion control quality detection method | |
| CN108285326B (en) | Green environment-friendly fly ash ceramsite and preparation method and application thereof | |
| CN112570432B (en) | Dechlorination method for coal-fired power plant desulfurization wastewater drying ash | |
| CN101806681A (en) | Optimal digestion method in waste colloidal particle heavy metal measurement | |
| CN103898535A (en) | Preparation raw material and method of black metal descaling agent | |
| CN204039201U (en) | A kind of device of waste hydrochloric acid containing iron comprehensive utilization of resources | |
| CN108276013A (en) | A kind of secondary aluminium scrap ash prepares the method and system of aluminium stone | |
| CN108912391A (en) | A kind of waste and old LDPE mixture recycling preparation process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201027 Address after: 510663 Room 501, 5 / F, building 9, No. 33, Kefeng Road, Guangzhou hi tech Industrial Development Zone, Guangdong Province Patentee after: Guogao high polymer material industry innovation center Co.,Ltd. Address before: 430056 No. 3, erudite Road, Wuhan economic and Technological Development Zone, Hubei Patentee before: WUHAN KINGFA SCI. & TECH. Co.,Ltd. Patentee before: WUHAN KINGFA TECHNOLOGY ENTERPRISE TECHNOLOGY CENTER Co.,Ltd. |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A cleaning method for alumina crucible of thermogravimetric instrument Effective date of registration: 20211217 Granted publication date: 20201023 Pledgee: Guangdong Development Bank Limited by Share Ltd. Guangzhou branch Pledgor: Guogao high polymer material industry innovation center Co.,Ltd. Registration number: Y2021980015517 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20230522 Granted publication date: 20201023 Pledgee: Guangdong Development Bank Limited by Share Ltd. Guangzhou branch Pledgor: Guogao high polymer material industry innovation center Co.,Ltd. Registration number: Y2021980015517 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A Cleaning Method for Alumina Crucible of Thermal Weight Loss Instrument Effective date of registration: 20230524 Granted publication date: 20201023 Pledgee: Guangdong Development Bank Limited by Share Ltd. Guangzhou branch Pledgor: Guogao high polymer material industry innovation center Co.,Ltd. Registration number: Y2023980041520 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |