CN1282602C - Purification method of kieselguhr filler - Google Patents
Purification method of kieselguhr filler Download PDFInfo
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- CN1282602C CN1282602C CN 200410060785 CN200410060785A CN1282602C CN 1282602 C CN1282602 C CN 1282602C CN 200410060785 CN200410060785 CN 200410060785 CN 200410060785 A CN200410060785 A CN 200410060785A CN 1282602 C CN1282602 C CN 1282602C
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- filler
- diatomaceous earth
- earth filler
- kieselguhr
- calcination
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Abstract
The present invention relates to a purification method of a kieselguhr filler. After the kieselguhr filler is washed by aid and organic solvents, the kieselguhr filler is continuously burnt in the temperature of 550 DEG C to 850 DEG C for 12 to 48 hours. The present invention solves the problem that the existing kieselguhr filler can not be repeatedly used after use because of containing impurity. The method of the present invention can effectively remove inorganic and organic impurities in the kieselguhr filler, the kieselguhr filler can be commonly and repeatedly used for 4 times, and the use cost is greatly saved.
Description
Technical field
The present invention relates to the purifying method of a kind of method of purification of filler, particularly a kind of diatomaceous earth filler.
Background technology
Matrix solid phase dispersion technology is a kind of sample-pretreating method commonly used in the Food Safety Analysis (pesticide residue, residue of veterinary drug, antibiotic remains in the food), diatomite is a critical material realizing this technology, it can adsorb moisture content and various interfering substance in the food samples, and interfering substance is separated with target compound (pesticide residue, residue of veterinary drug, antibiotic remains in the food).Because diatomite is attached has inhaled moisture content and interfering substance, if do not carry out purifying treatment, has just lost its use value.Now, employed diatomite all is dropped after use usually in the matrix solid phase dispersion technology, generally is considered as " disposable use " material by people.Because diatomite price comparison costliness, every kilogram is 5000 yuan, and major part is all from external import, if therefore can not regenerate and reuse diatomaceous earth filler, can cause very big waste.For many years, relevant researchist is studying the whole bag of tricks always.Existing method generally adopts acid to boil to remove impurity, and still this method poor effect can not effectively be removed impurity.Other relevant diatomite purifying method was not met report in the document at home and abroad yet.
Summary of the invention
Technical problem to be solved by this invention provides a kind of purifying method of diatomaceous earth filler, to remedy the deficiency of existing method.
Purifying method of the present invention may further comprise the steps:
(1), diatomaceous earth filler is washed with acid, washing the back water washs;
(2), will wash with volatile organic solvent after the above-mentioned diatomaceous earth filler drying;
(3), will carry out drying with the diatomaceous earth filler behind the organic solvent washing;
(4), the diatomaceous earth filler that drying is intact carries out calcination, calcination temperature is 750 ℃, calcination time is continuous 24 hours;
(5), the intact back of calcination adopts the water-bath cooling, coolant water temperature is below 10 ℃;
(6), carry out vacuum packaging after removing powder with 100 purpose filter sieve.
The purification process condition optimization is 750 ℃ of continuous calcinations 24 hours, volatile organic solvent preferred alcohol or acetone.
The contriver is through repeatedly experiment, successfully find out diatomaceous purifying method, in full accord through the diatomite of purifying treatment and new diatomaceous result of use, make diatomaceous earth filler become the material that " to reuse " by " disposable use ", improve the service efficiency of this material of diatomite, and reduced the cost of Food Safety Analysis.
Description of drawings
Fig. 1 is original diatomite gas-chromatography test pattern
Fig. 2 is used diatomite gas-chromatography test pattern
Fig. 3 is a used diatomite and through the gas-chromatography test pattern of present method after 750 ℃ of purifying treatment
Fig. 4 is through the gas-chromatography test pattern of present method after 550 ℃ of purifying treatment
Fig. 5 is through the gas-chromatography test pattern of present method after 600 ℃ of purifying treatment
Fig. 6 is through the gas-chromatography test pattern of present method after 700 ℃ of purifying treatment
Purify the evaluation of effect: to original diatomite, the diatomite that used and through the diatomite that had used of this method processing compare test as follows:
Above-mentioned 3 kinds of diatomite are respectively got 20g, are packed into respectively in the glass chromatography column, use 200mL The drip washing of the residual level of farming n-hexane, all coutroi velocity is 5mL/min, collect n-hexane drip washing liquid in Concentrate in the bottle. Concentrate to 1mL respectively, get 1 μ L concentrate gas chromatography combined with mass spectrometry Instrument is analyzed, and by observing instrument signal, judges.
Fig. 1 is original diatomite, after n-hexane drip washing, and the instrument signal of concentrate Showing does not have strong response peak substantially, shows on the original diatomite substantially not adsorb organic compound Matter.
The diatomite (without this method purified treatment) of Fig. 2 for using, after n-hexane drip washing, The instrument signal many places of concentrate demonstrate very strong response peak, show on the diatomite that used Absorption has a large amount of organic interfering materials.
The diatomite (through this method purified treatment) of Fig. 3 for using, after n-hexane drip washing, The instrument signal of concentrate shows does not have strong response peak substantially, shows through this method and processes use Substantially adsorb organic compound matter not on the diatomite of crossing is consistent with the situation of the diatomite that does not use.
From Fig. 4, Fig. 5, Fig. 6 analysis chart, can obviously find out, 550 ℃, 600 ℃, 700 ℃ are carried out after the calcination micro organic impurity being arranged still, and 750 ℃ then basic purification is clean. If excess Temperature or overlong time then become powder with tripolite filling material calcination fragmentation or calcination easily The end, impact is used.
Embodiment
Specify method of the present invention below in conjunction with embodiment:
(1), diatomaceous earth filler is washed with sulfuric acid or hydrochloric acid, washing the back water washs;
(2), will wash with ethanol or acetone after the above-mentioned diatomaceous earth filler drying;
(3), will volatilize with the diatomaceous earth filler behind ethanol or the washing with acetone, drying;
(4), the diatomaceous earth filler that drying is intact carries out calcination, calcination temperature is 750 ℃, calcination time is continuous 24 hours.
(5), the intact back of calcination adopts the water-bath cooling, coolant water temperature is below 10 ℃;
(6), carry out vacuum packaging after removing powder with 100 purpose filter sieve.
Calcination temperature selects 550 ℃, 600 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃ respectively, and calcination time selects 12 hours respectively, 24 hours, 36 hours, 48 hours.Prove through test-results; temperature is 550 ℃, 600 ℃, 700 ℃; also residual when the time is shorter than 24 hours have an organic impurity; temperature is 800 ℃, 850 ℃; time is under 36 or 48 hours the condition; diatomaceous earth filler is broken into fine particle or powder, and inconvenience is used, and determines that thus best purification condition is 750 ℃ of continuous calcinations 24 hours.Through the purifying treatment of the inventive method, can effectively remove the inorganic and organic impurity in the diatomaceous earth filler, diatomaceous earth filler generally can be reused 4 times, saved use cost greatly.
Claims (2)
1, a kind of purifying method of diatomaceous earth filler, it may further comprise the steps:
(1), diatomaceous earth filler is washed with acid, washing the back water washs;
(2), will wash with volatile organic solvent after the above-mentioned diatomaceous earth filler drying;
(3), will carry out drying with the diatomaceous earth filler behind the organic solvent washing;
(4), the diatomaceous earth filler that drying is intact carries out calcination, calcination temperature is 750 ℃, calcination time is continuous 24 hours;
(5), the intact back of calcination adopts the water-bath cooling, coolant water temperature is below 10 ℃;
(6), carry out vacuum packaging after removing powder with 100 purpose filter sieve.
2, according to the purifying method of a kind of diatomaceous earth filler of claim 1, wherein volatile organic solvent is ethanol or acetone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410060785 CN1282602C (en) | 2004-08-31 | 2004-08-31 | Purification method of kieselguhr filler |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410060785 CN1282602C (en) | 2004-08-31 | 2004-08-31 | Purification method of kieselguhr filler |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1618734A CN1618734A (en) | 2005-05-25 |
| CN1282602C true CN1282602C (en) | 2006-11-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200410060785 Expired - Fee Related CN1282602C (en) | 2004-08-31 | 2004-08-31 | Purification method of kieselguhr filler |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1282602C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| HUP1000547A2 (en) | 2010-10-12 | 2012-07-30 | Egis Gyogyszergyar Nyrt | Process to produce suitable auxiliary material for use in pharmaceutical industry |
| CN104326476A (en) * | 2014-10-16 | 2015-02-04 | 桂林新竹大自然生物材料有限公司 | Method for preparing high-quality diatomite based on supersonic wave effect by hydrochloric acid method |
| CN104310411A (en) * | 2014-10-16 | 2015-01-28 | 桂林新竹大自然生物材料有限公司 | Method for preparing high-quality diatomite by oscillation-based hydrochloric acid process |
| CN109577076A (en) * | 2018-12-26 | 2019-04-05 | 江苏理文造纸有限公司 | A kind of filler and preparation method thereof for liner board |
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2004
- 2004-08-31 CN CN 200410060785 patent/CN1282602C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1618734A (en) | 2005-05-25 |
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