CN1721058A - Adsorption material for removing copper and lead from plant medicine and preparation method thereof - Google Patents
Adsorption material for removing copper and lead from plant medicine and preparation method thereof Download PDFInfo
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- CN1721058A CN1721058A CN 200510013556 CN200510013556A CN1721058A CN 1721058 A CN1721058 A CN 1721058A CN 200510013556 CN200510013556 CN 200510013556 CN 200510013556 A CN200510013556 A CN 200510013556A CN 1721058 A CN1721058 A CN 1721058A
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Abstract
The present invention relates to absorption material and its preparation method to remove the cupper and lead in plant drug system and belongs to trace weight metal technique. The material is magnesium aluminate hydrotalcite layer-pole compound power with carried mass 0-2% of one or more kinds of zirconium, cerium, argent and gadolinium. The preparation method comprises steps as listed: prepare magnesium aluminate hydrotalcite with Al(OH)3 and Mg(NO3)2, prepare titanium pole agent and the treatment for all metallic ion. The advantage of this invention lies on that the absorption material can be used at room temperature with good effect; the limit absorption depth is 50ppb; its preparation method and process is simple.
Description
Technical field
The present invention relates to a kind of copper in the autonomic drug system and plumbous sorbing material and preparation method thereof removed, belong to the Chinese medicine system trace heavy metal technology of removing
Background technology
At present, Chinese medicine and natural drug industry with Chinese traditional culture characteristic and unique advantage are faced with good development opportunity and challenge, " the green industry standard of plant extracts and preparation thereof " makes respective specified to heavy metal indexs such as Cu, Pb, Hg, Cd, As in domestic Chinese medicine and the autonomic drug product, require Pb content less than 5.0ppm, Cu content is less than 20ppm.The trace heavy metal subject matter that problem has become influences autonomic drug quality and security that exceeds standard, numerous traditional products still can not meet international medical standard and requirement fully.Therefore, develop a class to trace copper and the plumbous sorbing material that proprietary adsorption effect is arranged, and extract at autonomic drug, concentrate, process such as purifying is applied, copper and lead content in the control autonomic drug extract make China's traditional Chinese medicine and autonomic drug industry thereof develop to standardization, modernization, internationalization direction.
Summary of the invention
The object of the present invention is to provide a kind of copper in the autonomic drug system and plumbous sorbing material and preparation method thereof removed, this sorbing material is to the copper in the autonomic drug system and plumbous have a good adsorption performance, and its preparation method is simple.
The present invention is realized by following technical proposals.A kind of copper in the autonomic drug system and plumbous sorbing material removed is characterized in that this material is a magnalium hydrotalcite layer-pillared compound powder, and load quality is one or both or three kinds or four kinds of zirconium, cerium, silver and the gadolinium of 0.1-2% on it.
Above-mentioned sorbing material preparation method is characterized in that comprising the following steps:
1. concentration is the Al (OH) of 0.1-5mol/L
3Solution and concentration are the Mg (NO of 0.1-5mol/L
3)
2Mix down at 20-30 ℃, stirred 2 hours, left standstill 5-12 hour, filter, spend deionised water 3 times, obtain magnalium hydrotalcite.
2. with TiCl
4Be dissolved in the HCl solution of 0.1-5mol/L concentration, then through diluting to such an extent that contain the pillaring solution that Ti concentration is 0.4-0.9mol/L.
3. the magnalium hydrotalcite that step 1 is obtained is according to the ratio formulated suspension of quality 1-5%, and the average grain diameter of magnalium hydrotalcite is the 5-50 micron, pillaring solution slowly is added dropwise to institute joins in the suspension, stirs while dripping.After stirring end, suspension is placed pressure vessel, under 0-5MPa pressure and 10-300 ℃ of temperature conditions, left standstill 0-48 hour respectively.Leach then, under 100-120 ℃ of condition, dry.
4. sample is placed muffle furnace, any under room temperature-860 ℃ condition or the heating of a plurality of temperature spot 1-2 hour, with the stove cooling, being ground to granularity is the 80-200 order.
5. the hydrotalcite with roasting is immersed in respectively under room temperature in zirconyl chloride solution, liquor argenti nitratis ophthalmicus, cerous nitrate solution or the gadolinium oxide solution of 0.01mol/L-0.5mol/L, soaks 1-48 hour, filters and takes out.
6. above sample was shone 1-60 minute oven dry under the microwave of 370W.
7. the hydrotalcite that step 6 is obtained places muffle furnace to heat 1-8 hour down in 300-400 ℃, makes sorbing material.
8. if imvite is dipped in the liquor argenti nitratis ophthalmicus in 5 set by step, add quality 5-10% formaldehyde, soaks after 1-48 hour, left standstill 5 hours in 70-90 ℃ of following lucifuge, to filter and take out, oven dry must contain the silver-colored sorbing material of simple substance.
The invention has the advantages that sorbing material can use at ambient temperature, result of use is good, removes copper and the plumbous good effect that has in the autonomic drug system, can reach the effect of degree of depth absorption, limit adsorption concentration 50ppb.
The specific embodiment
Embodiment 1:
With concentration is the Al (OH) of 0.1-5mol/L
3Solution and concentration are the Mg (NO of 0.1-5mol/L
3)
2Mix down at 20-30 ℃, stirred 2 hours, left standstill 5-12 hour, filter, spend deionised water 3 times, obtain magnalium hydrotalcite.TiCl just
4Be dissolved in the HCl solution of 3mol/L, then through diluting to such an extent that Ti concentration is 0.86mol/L; HCl concentration is the pillaring solution of 0.7mol/L, in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% (wt) hydrotalcite suspension that is made under constantly stirring, and the average grain diameter of hydrotalcite is the 5-50 micron.After stirring, leave standstill 12h, Separation of Solid and Liquid is washed for several times to not having the Cl ion and oven dry under 100 ℃ with distilled water simultaneously again.In 600 ℃-650 ℃ following calcining 5h, get the titanium pillared hydrotalcite at last, the concentration of titanium pillared hydrotalcite with 4% (wt) be immersed in the ammonium copper sulfate solution of 0.1mol/L through being ground to the 80-200 order, leave standstill 12h after, filtering, dry in 100 ℃.Result of study shows that sorbing material has good adsorption effect to copper and lead in the water and in the ethanolic solution.
Embodiment 2:
With concentration is the Al (OH) of 0.1-5mol/L
3Solution and concentration are the Mg (NO of 0.1-5mol/L
3)
2Mix down at 20-30 ℃, stirred 2 hours, left standstill 5-12 hour, filter, spend deionised water 3 times, obtain magnalium hydrotalcite.With TiCl
4Be dissolved in the HCl solution of 3mol/L, then through diluting to such an extent that Ti concentration is 0.86mol/L; HCl concentration is the pillaring solution of 0.7mol/L, in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% (wt) hydrotalcite suspension that is made under constantly stirring, and the average grain diameter of hydrotalcite is the 5-50 micron.After 3 hours stirring, suspension is inserted in the high-pressure bottle airtight, be to leave standstill 12h under 300 ℃ of conditions in temperature, suspension takes out after Separation of Solid and Liquid, simultaneously with the distilled water washing for several times to not having the Cl ion and in 100 ℃ of oven dry down.Calcine 5h down in 600 ℃-650 ℃ at last, get the titanium pillared hydrotalcite through being ground to the 80-200 order, the concentration of titanium pillared hydrotalcite with 4% (wt) is immersed in the zirconyl chloride solution of 0.1mol/L, after leaving standstill 12h, filtering, in 370 watts of micro-wave oven internal radiations 10 minutes, in 120 ℃ of oven dry down, make sorbing material again.Result of study shows that sorbing material has good adsorption effect to copper and lead in the water and in the ethanolic solution.
Claims (2)
1. remove copper in the autonomic drug system and plumbous sorbing material for one kind, it is characterized in that this material is a magnalium hydrotalcite layer-pillared compound powder, load quality is one or both or three kinds or four kinds of zirconium, cerium, silver and the gadolinium of 0-2% on it.
2. the preparation method by the described sorbing material of claim 1 is characterized in that comprising the following steps:
1). with concentration is the Al (OH) of 0.1-5mol/L
3Solution and concentration are the Mg (NO of 0.1-5mol/L
3)
2Mix down at 20-30 ℃, stirred 2 hours, left standstill 5-12 hour, filter, spend deionised water 3 times, obtain magnalium hydrotalcite;
2). with TiCl
4Be dissolved in the HCl solution of 0.1-5mol/L concentration, then through diluting to such an extent that contain the pillaring solution that Ti concentration is 0.4-0.9mol/L;
3). with rapid 1) magnalium hydrotalcite that obtains is according to the ratio formulated suspension of quality 1-5%, the average grain diameter of magnalium hydrotalcite is the 5-50 micron, pillaring solution slowly is added dropwise to institute joins in the suspension, stir while dripping, after stirring end, suspension is placed pressure vessel, under 0-5MPa pressure and 10-300 ℃ of temperature conditions, leave standstill respectively and leached then in 0-48 hour, under 100-120 ℃ of condition, dry;
4). sample is placed muffle furnace, any under room temperature-860 ℃ condition or the heating of a plurality of temperature spot 1-2 hour, with the stove cooling, being ground to granularity is the 80-200 order;
5). the hydrotalcite of roasting is immersed in respectively under room temperature in zirconyl chloride solution, liquor argenti nitratis ophthalmicus, cerous nitrate solution or the gadolinium oxide solution of 0.01mol/L-0.5mol/L, soaked 1-48 hour, filter and take out;
6). above sample was shone 1-60 minute oven dry under the microwave of 370W;
7). the hydrotalcite that step 6) is obtained places muffle furnace to heat 1-8 hour down in 300-400 ℃, makes sorbing material;
8) if. set by step 5) in imvite is dipped in the liquor argenti nitratis ophthalmicus, add quality 5-10% formaldehyde, soaks after 1-48 hour, left standstill 5 hours in 70-90 ℃ of following lucifuge, filter and take out, oven dry must contain the silver-colored sorbing material of simple substance.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100135565A CN100382886C (en) | 2005-05-26 | 2005-05-26 | Adsorption material for removing copper and lead from plant medicine and preparation method thereof |
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| CNB2005100135565A CN100382886C (en) | 2005-05-26 | 2005-05-26 | Adsorption material for removing copper and lead from plant medicine and preparation method thereof |
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| CN1721058A true CN1721058A (en) | 2006-01-18 |
| CN100382886C CN100382886C (en) | 2008-04-23 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837286A (en) * | 2010-05-20 | 2010-09-22 | 浙江工业大学 | Hydrotalcite-like compound-based magnesium-titanium-aluminum composite oxide catalyst and application thereof |
| CN104474739A (en) * | 2014-12-04 | 2015-04-01 | 上海绿强新材料有限公司 | Application of molecular sieve adsorption material in removing of traditional Chinese medicine heavy metal |
| CN106629968A (en) * | 2016-11-03 | 2017-05-10 | 张静 | Preparation method of adsorption material used for removing heavy metal copper in waste water |
| WO2020211708A1 (en) * | 2019-04-16 | 2020-10-22 | 马德君 | Use of anionic clay in preparing lead-removing medicament |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5424993B2 (en) * | 1972-03-02 | 1979-08-24 | ||
| JPS5049181A (en) * | 1973-08-31 | 1975-05-01 | ||
| ES2229105T3 (en) * | 2001-02-09 | 2005-04-16 | Akzo Nobel N.V. | IN SITU CONFORMED ELEMENTS CONTAINING CRYSTAL ANIONIC CLAY. |
| CN1507944A (en) * | 2002-12-18 | 2004-06-30 | 北京化工大学 | Method for clean synthesizing magnesite-alumina hydrotalcite |
| CN1566260A (en) * | 2003-07-01 | 2005-01-19 | 北京化工大学 | Photochromic nitrate type hydrotalcite and method for producing the same |
| CN1234808C (en) * | 2004-03-11 | 2006-01-04 | 天津大学 | Desulfate adsorbing agent for deep purifying sulfide in fuel oil and preparation process thereof |
-
2005
- 2005-05-26 CN CNB2005100135565A patent/CN100382886C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837286A (en) * | 2010-05-20 | 2010-09-22 | 浙江工业大学 | Hydrotalcite-like compound-based magnesium-titanium-aluminum composite oxide catalyst and application thereof |
| CN104474739A (en) * | 2014-12-04 | 2015-04-01 | 上海绿强新材料有限公司 | Application of molecular sieve adsorption material in removing of traditional Chinese medicine heavy metal |
| CN104474739B (en) * | 2014-12-04 | 2016-08-31 | 上海绿强新材料有限公司 | The application in removing traditional Chinese medicine heavy metal of a kind of molecular sieve adsorption material |
| CN106629968A (en) * | 2016-11-03 | 2017-05-10 | 张静 | Preparation method of adsorption material used for removing heavy metal copper in waste water |
| WO2020211708A1 (en) * | 2019-04-16 | 2020-10-22 | 马德君 | Use of anionic clay in preparing lead-removing medicament |
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| CN100382886C (en) | 2008-04-23 |
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