CN1704156A - Adsorbent for deeply purifying trace quantity arsenic in plant extract and preparation method thereof - Google Patents
Adsorbent for deeply purifying trace quantity arsenic in plant extract and preparation method thereof Download PDFInfo
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- CN1704156A CN1704156A CN 200410019472 CN200410019472A CN1704156A CN 1704156 A CN1704156 A CN 1704156A CN 200410019472 CN200410019472 CN 200410019472 CN 200410019472 A CN200410019472 A CN 200410019472A CN 1704156 A CN1704156 A CN 1704156A
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Abstract
The invention discloses arsenic sorbent and it's preparing method which is used in depth purified plant abstraction in the field of detaching the arsenic impurity of plant abstraction. The sorbent uses layer column compound of montmorillonite or hydrotacite as mother material and compounds with the powder of titanium, cerium, iron, gadolinium and silver. The preparing method comprises the following steps: preparing titanium column agent, preparing the floating liquid of montmorillonite or hydrotacite and mixing them, obtaining striping arsenic sorbent by roasting, sinking, filtering, and positing the yield at low temperature plasma with non-microwave irradiation, at last sinking it in the solution.
Description
Technical field
The present invention relates to a kind of sorbent material that is used for deep purifying plant milk extract trace arsenic and preparation method thereof, belong to the arsenic impurities technology in the plant milk extract of removing.
Background technology
Arsenic is one of ubiquitous heavy metal in the plant amedica, has proposed the controlling index at different varieties both at home and abroad, and " herbal medicine of doing (arsenic) is 5 * 10 for the European Community and member states's requirement thereof
-6(massfraction) ", arsenic content is lower than 2 * 10 in the Tianjin traditional Chinese medicine enterprise proposition patent medicine product
-6(massfraction).Plant amedica is in preparation process, and the spissated while of effective constituent, trace elements such as arsenic also almost are by the equal proportion enrichment.In general, the concentration ratio of plant amedica extract and final product is 30～100, and unit processes such as dearsenification can only be finished before concentrating, and calculate that by this concentration of arsenic must be controlled at 2 * 10 in extract
-8～7 * 10
-8(massfraction).Therefore, the total content of arsenic in the controlling plant medicine is realized quality control standardization, and its core is to develop at trace ionic sorbing material.
The problem that arsenic in the plant amedica product is exceeded standard, be reported in and adopt combination macroporous adsorbent resin or neutral alumina to make sorbent material in the course of processing, chitosan is made technique means such as finings and supercritical extraction, these methods have certain effect to the removal of heavy metal ion such as Hg, As, but poor selectivity, and can not handle the ion that exceeds standard of trace concentration.Therefore, a synthetic class selectivity height, loading capacity are big, chemistry and Heat stability is good, the trace micro anion is had adsorbing arsenic removal ionic sieve, trace arsenic in the plant milk extract is carried out effective separation and Extraction, can effectively solve the problem that trace harmful elements exceeds standard in the different plant amedica kinds.
Summary of the invention
The object of the present invention is to provide a kind of sorbent material that is used for deep purifying plant milk extract trace arsenic and preparation method thereof, this adsorbents adsorb amount height, the preparation method is simple.
The present invention is realized by following technical proposals, is used for the sorbent material of deep purifying plant milk extract trace arsenic, it is characterized in that, and be base material with the layer-pillared compound of polynite or hydrotalcite, the powder of composite titanium, cerium, iron, gadolinium and silver on it.
Above-mentioned dearsenification preparation of adsorbent method is adopting montmorillonite or hydrotalcite, utilizes the interface package technique, and binding plasma technology and microwave irradiation technology are prepared from, and it is characterized in that comprising following process:
1, with TiCl
4Being dissolved in concentration is in 0.1～mol/LHCl solution, and thin up must contain the pillaring solution that Ti concentration is 0.4-0.9mol/L then.
2, with polynite or hydrotalcite according to the ratio formulated suspension of 1～5wt%, pillaring solution slowly is added dropwise in institute's formulated suspension, stir while dripping.After stirring end, suspension is placed container, under 0～5MPa pressure and 10～180 ℃ of temperature condition, left standstill 0～48 hour.Leach then, under 100～120 ℃ of conditions, dry.
3, sample is placed muffle furnace, any temperature section under 20～860 ℃ of conditions or the heating of a plurality of temperature section 1～2 hour are cooled off with furnace temperature then.
4, polynite or the hydrotalcite with roasting is immersed in respectively under room temperature in 0.01mol/L～0.5mo liquor ferri trichloridi, silver nitrate solution, cerous nitrate solution or the gadolinium oxide solution, soaked 1～48 hour, filter and take out, sample was placed low-temperature plasma 1～60 minute, under the microwave of 300～400W, shine oven dry in 1～60 minute then, place muffle furnace to heat down again and made the dearsenification sorbent material in 1～8 hour in 300～400 ℃; Or after will placing the sample taking-up of low-temperature plasma, add in 5～10wt% formaldehyde solution, soak after 1～48 hour, left standstill 1～5 hour in 70～90 ℃ of following lucifuges, filter and take out oven dry, get the dearsenification sorbent material.
The invention has the advantages that can use at ambient temperature, result of use is good, have function trace arsenic deep purifying in the plant milk extract.
Embodiment
Embodiment 1:
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/ polynite=20meq/g or in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% polynite or hydrotalcite suspension that are made under constantly stirring, after stirring, in container, leave standstill 12h 2MPa and 100 ℃, solid-liquid separation again, simultaneously with distilled water wash for several times to not having the Cl ion and in 100 ℃ of oven dry down.At last in 600 ℃～650 ℃ following calcining 5h, through grind the titanium pillared montmorillonite, titanium pillared montmorillonite or titanium pillared hydrotalcite are immersed in respectively in the liquor ferri trichloridi of 0.1mol/L with 4% concentration, leave standstill 12h after, after filtration, dry in 100 ℃.Result of study shows that the dearsenification sorbent material has good adsorption effect to trace arsenic in the plant milk extract.
Embodiment 2:
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/ polynite=20meq/g or in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% polynite or hydrotalcite suspension that are made under constantly stirring, after stirring, in container, leave standstill 10h 3MPa and 120 ℃, solid-liquid separation again, simultaneously with distilled water wash for several times to not having the Cl ion and in 100 ℃ of oven dry down.Calcine 5h down in 600 ℃～650 ℃ at last, through grind titanium pillared montmorillonite or titanium pillared hydrotalcite, titanium pillared montmorillonite or titanium pillared hydrotalcite are immersed in respectively in the silver nitrate solution of 0.1mol/L with 4% concentration, leave standstill 12h after, filtering, in 370 watts of microwave oven internal radiations 10 minutes.Result of study shows that the dearsenification sorbent material has good adsorption effect to trace arsenic in the plant milk extract.
Claims (2)
1, a kind of sorbent material that is used for deep purifying plant milk extract trace arsenic is characterized in that: this sorbent material is a base material for the layer-pillared compound with polynite or hydrotalcite, the powder of composite titanium, cerium, iron, gadolinium and silver on it.
2, a kind of by the described dearsenification preparation of adsorbent of claim 1 method, be to adopt with polynite or hydrotalcite, utilize the interface package technique, binding plasma technology and microwave irradiation technology are prepared from, and it is characterized in that comprising following process:
(1) with TiCl
4Being dissolved in concentration is in 0.1～mol/L HCl solution, and thin up must contain the pillaring solution that Ti concentration is 0.4-0.9mol/L then;
(2) with polynite or hydrotalcite according to the ratio formulated suspension of 1～5wt%, pillaring solution slowly is added dropwise in institute's formulated suspension, stir while dripping.After stirring end, suspension is placed container, under 0～5MPa pressure and 10～180 ℃ of temperature condition, left standstill 0～48 hour, leach then, under 100～120 ℃ of conditions, dry;
(3) sample is placed muffle furnace, any temperature section under 20～860 ℃ of conditions or the heating of a plurality of temperature section 1～2 hour are cooled off with furnace temperature then;
(4) polynite or the hydrotalcite with roasting is immersed in respectively under room temperature in 0.01mol/L～0.5mo liquor ferri trichloridi, silver nitrate solution, cerous nitrate solution or the gadolinium oxide solution, soaked 1～48 hour, filter and take out, sample was placed low-temperature plasma 1～60 minute, under the microwave of 300～400W, shine oven dry in 1～60 minute then, place muffle furnace to heat down again and made the dearsenification sorbent material in 1～8 hour in 300～400 ℃; After maybe will placing the sample of low-temperature plasma to take out, add in 5～10wt% formaldehyde solution, soaks after 1～48 hour,, filter and take out oven dry, get the dearsenification sorbent material in quiet 1～5 hour of 70～90 ℃ of following lucifuges.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100194728A CN100455346C (en) | 2004-06-04 | 2004-06-04 | Adsorbent for deeply purifying trace quantity arsenic in plant extract and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100194728A CN100455346C (en) | 2004-06-04 | 2004-06-04 | Adsorbent for deeply purifying trace quantity arsenic in plant extract and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1704156A true CN1704156A (en) | 2005-12-07 |
| CN100455346C CN100455346C (en) | 2009-01-28 |
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|---|---|---|---|
| CNB2004100194728A Expired - Fee Related CN100455346C (en) | 2004-06-04 | 2004-06-04 | Adsorbent for deeply purifying trace quantity arsenic in plant extract and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011042167A3 (en) * | 2009-10-09 | 2011-07-21 | Philip Morris Products S.A. | Methods for removing heavy metals from aqueous extracts of tobacco |
| CN101648130B (en) * | 2009-06-02 | 2012-10-24 | 清华大学 | Preparing method of titanium-rare earth composite adsorbent capable of efficiently removing arsenic |
| CN103169738A (en) * | 2013-03-28 | 2013-06-26 | 宁波立华植物提取技术有限公司 | Method for removing heavy metal from ganoderma extract |
| CN106673111A (en) * | 2017-01-10 | 2017-05-17 | 苏州大学 | Method for treating selenate radical containing waste water |
-
2004
- 2004-06-04 CN CNB2004100194728A patent/CN100455346C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101648130B (en) * | 2009-06-02 | 2012-10-24 | 清华大学 | Preparing method of titanium-rare earth composite adsorbent capable of efficiently removing arsenic |
| WO2011042167A3 (en) * | 2009-10-09 | 2011-07-21 | Philip Morris Products S.A. | Methods for removing heavy metals from aqueous extracts of tobacco |
| CN103169738A (en) * | 2013-03-28 | 2013-06-26 | 宁波立华植物提取技术有限公司 | Method for removing heavy metal from ganoderma extract |
| CN103169738B (en) * | 2013-03-28 | 2015-01-28 | 宁波立华植物提取技术有限公司 | Method for removing heavy metal from ganoderma extract |
| CN106673111A (en) * | 2017-01-10 | 2017-05-17 | 苏州大学 | Method for treating selenate radical containing waste water |
| CN106673111B (en) * | 2017-01-10 | 2020-09-08 | 苏州大学 | Method for treating wastewater containing selenate |
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| Publication number | Publication date |
|---|---|
| CN100455346C (en) | 2009-01-28 |
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Granted publication date: 20090128 Termination date: 20210604 |