CN100455346C - 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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- CN100455346C CN100455346C CNB2004100194728A CN200410019472A CN100455346C CN 100455346 C CN100455346 C CN 100455346C CN B2004100194728 A CNB2004100194728 A CN B2004100194728A CN 200410019472 A CN200410019472 A CN 200410019472A CN 100455346 C CN100455346 C CN 100455346C
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- hydrotalcite
- titanium
- arsenic
- adsorbent
- absorbent
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Abstract
The present invention discloses an absorbent for deeply purifying trace quantity arsenic in plant extracts and a preparation method thereof, which belongs to a technique for removing arsenic impurities from plant extracts. The absorbent takes layer post compounds of montmorillonite or hydrotalcite as base materials, and the powder of titanium, cerium, iron, gadolinium and silver are compounded on the base materials. The preparation method comprises the processes: a titanium column agent is prepared, the suspension of the montmorillonite or the hydrotalcite are prepared, the titanium column agent and the suspension are mixed, and the dearsenization absorbent is prepared by products of the mixture via calcination, soaking in solution, filtration, arrangement in low-temperature plasma and microwave irradiation; or the dearsenization absorbent is prepared by the products via calcination, soaking in solution, filtration, arrangement in low-temperature plasma and solution soaking without microwave irradiation. The absorbent has the advantage that the absorbent can be used at room temperature and has good use effects and a purifying function for deeply purifying the trace amount arsenic from the plant extracts.
Description
Technical field
The present invention relates to a kind of adsorbent that is used for deep purifying plant extracts trace arsenic and preparation method thereof, belong to the arsenic impurities technology in the plant extracts of removing.
Background technology
Arsenic is one of ubiquitous heavy metal in the autonomic drug, has proposed the control index at different cultivars both at home and abroad, and " herbal medicine of doing (arsenic) is 5 * 10 for the European Community and member state's requirement thereof
-6(mass fraction) ", arsenic content is lower than 2 * 10 in the Tianjin traditional Chinese medicine enterprise proposition patent medicine product
-6(mass fraction).Autonomic drug is in preparation process, and when active ingredient concentrated, trace elements such as arsenic also almost were by the equal proportion enrichment.In general, the cocnentration factor of autonomic drug extract and end 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(mass fraction).Therefore, the total content of arsenic is realized quality control standardization in the control autonomic drug, and its core is the sorbing material exploitation at the trace ion.
The problem that arsenic in the autonomic drug product is exceeded standard, be reported in and adopt combination macroporous absorbent resin or neutral alumina to make adsorbent in the process, shitosan is made technological means such as fining agent and supercritical extract, 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, adsorption 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 extracts is carried out effective separation and Extraction, can effectively solve the problem that trace harmful elements exceeds standard in the different autonomic drug kinds.
Summary of the invention
The object of the present invention is to provide a kind of adsorbent that is used for deep purifying plant extracts 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 adsorbent of deep purifying plant extracts trace arsenic, it is characterized in that: this adsorbent is a base material for the layer-pillared compound with imvite or hydrotalcite, the powder of composite titanium 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 the 3mol/L HCl solution, and must to contain Ti concentration be that 0.86mol/L and HCl concentration are the pillaring solution of 0.7mol/L to thin up then.
2, in Ti/ imvite=20meq/g or in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% imvite that is being made into or hydrotalcite suspension, after stirring, under 3MPa pressure and 120 ℃ of temperature conditions, left standstill 10～12 hours, Separation of Solid and Liquid is washed for several times to not having the Cl ion and drying down in 100 ℃ with distilled water simultaneously again.
3, sample is placed muffle furnace, calcining is 5 hours under 600～650 ℃ of conditions, then with furnace temperature cooling, through grind titanium pillared montmorillonite or titanium pillared hydrotalcite;
4, titanium pillared montmorillonite that step 3 is made or titanium pillared hydrotalcite soak in the liquor argenti nitratis ophthalmicus of 0.1mol/L with 4% concentration, after leaving standstill 12 hours, filter to take out, then under the microwave of 370W irradiation dried in 10 minutes the dearsenification adsorbent of composite titanium and silver.
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 extracts.
The specific 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/ imvite=20meq/g or in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% imvite or hydrotalcite suspension that are made under constantly stirring, after stirring, in 2MPa and 100 ℃ of containers, leave standstill 12h, Separation of Solid and Liquid is washed for several times to not having the Cl ion and drying down in 100 ℃ with distilled water simultaneously again.At last in 600 ℃～650 ℃ following calcining 5h, through grind the titanium pillared montmorillonite, titanium pillared montmorillonite or titanium pillared hydrotalcite are immersed 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 adsorbent has good adsorption effect to trace arsenic in the plant extracts.
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/ imvite=20meq/g or in Ti/ hydrotalcite=20meq/g ratio pillaring solution is slowly dripped in 2% imvite or hydrotalcite suspension that are made under constantly stirring, after stirring, in container, leave standstill 10h 3MPa and 120 ℃, Separation of Solid and Liquid is washed for several times to not having the Cl ion and drying down in 100 ℃ with distilled water simultaneously again.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 the liquor argenti nitratis ophthalmicus of 0.1mol/L with 4% concentration, leave standstill 12h after, filtering, in 370 watts of micro-wave oven internal radiations 10 minutes.Result of study shows that the dearsenification adsorbent has good adsorption effect to trace arsenic in the plant extracts.
Claims (1)
1. preparation of adsorbent method that is used for deep purifying plant extracts trace arsenic, described adsorbent is a base material for the layer-pillared compound with imvite or hydrotalcite, composite titanium and silver-colored powder it on is characterized in that comprising following process:
(1) with TiCl
4Being dissolved in concentration is in the HCl solution of 3mol/L, and must to contain Ti concentration be that 0.86mol/L and HCl concentration are the pillaring solution of 0.7mol/L to thin up then;
(2) in Ti/ imvite=20meq/g or pillaring solution slowly is added dropwise in 2% imvite or hydrotalcite suspension that is made in Ti/ hydrotalcite=20meq/g ratio, stir while dripping, under 3MPa pressure and 120 ℃ of temperature conditions, left standstill 10 hours afterwards, Separation of Solid and Liquid is washed for several times to not having the Cl ion and drying down in 100 ℃ with distilled water simultaneously again;
(3) sample is placed muffle furnace, calcining is 5 hours under 600～650 ℃ of conditions, then with furnace temperature cooling, through grind titanium pillared montmorillonite or titanium pillared hydrotalcite;
(4) titanium pillared montmorillonite that step (3) is made or titanium pillared hydrotalcite are soaked in respectively in the liquor argenti nitratis ophthalmicus of 0.1mol/L with 4% concentration, after leaving standstill 12 hours, filter and take out, irradiation oven dry in 10 minutes under the microwave of 370W then makes the dearsenification adsorbent of montmorillonite Composite titanium and silver or the dearsenification adsorbent of hydrotalcite composite titanium and silver.
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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1704156A CN1704156A (en) | 2005-12-07 |
| CN100455346C true 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 (1)
| 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 |
Families Citing this family (3)
| 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 |
| 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 |
| CN106673111B (en) * | 2017-01-10 | 2020-09-08 | 苏州大学 | Method for treating wastewater containing selenate |
-
2004
- 2004-06-04 CN CNB2004100194728A patent/CN100455346C/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
|---|
| Selective Catalytic Reduction of NitrogenOxides by Ammonia over Fe3+-Exchanged Tio2-Pillared ClayCatalysts. R.Q.Long.Journal of Catalysis,No.第186期. 1999 |
| Selective Catalytic Reduction of NitrogenOxides by Ammonia over Fe3+-Exchanged Tio2-Pillared ClayCatalysts. R.Q.Long.Journal of Catalysis,No.第186期. 1999 * |
| 用TiO2-Ag-改性膨润土复合催化剂光催化氧化处理染料废水. 陈集，罗建生等.环境技术，第6卷. 2002 |
| 用TiO2-Ag-改性膨润土复合催化剂光催化氧化处理染料废水. 陈集，罗建生等.环境技术，第6卷. 2002 * |
Cited By (1)
| 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 |
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| CN1704156A (en) | 2005-12-07 |
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