CN102132799A - Method for removing residual heavy metal in rice - Google Patents
Method for removing residual heavy metal in rice Download PDFInfo
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- CN102132799A CN102132799A CN201110050464XA CN201110050464A CN102132799A CN 102132799 A CN102132799 A CN 102132799A CN 201110050464X A CN201110050464X A CN 201110050464XA CN 201110050464 A CN201110050464 A CN 201110050464A CN 102132799 A CN102132799 A CN 102132799A
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- carbon dioxide
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Abstract
The invention discloses a method for removing residual heavy metal in rice, which uses supercritical fluid as an extractant to effectively remove the residual heavy metal in rice. The shape, nutrition substances and flavor of the rice can be maintained during removing of the heavy metal, no secondary pollution can be caused to the rice during the removing of the heavy metal, and harmful wastes to the environment can not generate as well.
Description
Technical field
The present invention relates to the method for a kind of agricultural product and grain deep processing, relate in particular to a kind of method that removes remaining heavy metal in the rice.
Background technology
Heavy metal remnants are major issues of food security.In recent years, because being subjected to the pollution of each heavy metal species, atmosphere, water body and soil caused the serious problems of heavy metal remnants in the cereal product.The residual removal technical difficulty of micro heavy is big in the cereal products such as rice, the standard increasingly stringent.Requirement is for cereal products such as rice, and the process of removing heavy metal can not cause secondary pollution to grain, can not damage nutrition, form and the outward appearance of cereal product.Existing removal method all can cause secondary pollution to food when removing heavy metal, and all can damage rice.All do not see the relevant relevant report that removes remaining heavy metal applicable technology in the rice at present both at home and abroad.
Summary of the invention
Supercritical fluid is meant that temperature and pressure surpasses the material of its vapour-liquid critical-temperature and critical pressure state.Supercritical fluid has the characteristics of liquids and gases concurrently: have the dissolubility of liquid and the diffusivity of gas, density is bigger than gas, and viscosity ratio liquid is little, and surface tension is zero.The density of supercritical fluid is very sensitive to temperature, pressure, increases with the rising of pressure, reduces with the rising of temperature; Its solvability strengthens with the increase of density.Supercritical fluid is the fine solvent of unique properties.Have following characteristics with supercritical fluid as the supercritical liquid extraction technique of extractant: can regulate its solvability by changing the temperature, pressure of fluid to solute, thus the selective extraction desirable ingredients; Can realize separating step integrated of solvent extraction, solute and the solvent of solute, technology is simple, and energy consumption is low, and operating cost is low; Can realize the separation of multiple material selectively by the multi-stage separation of different temperatures and pressure; Because the surface tension of supercritical fluid is zero, has very high diffusivity, be easy to infiltrate in the micropore of extract, so mass transfer rate is fast, the extraction efficiency height; Supercritical fluid media realizes recycling easily, and is environmentally friendly.Supercritical carbon dioxide is first-selected good extraction fluid, and it has following characteristics: critical-temperature of carbon dioxide (31.1 ℃) and critical pressure (73.8kg/cm
2) relatively low, realize supercriticality easily; Because its critical-temperature is low, can protect the thermal sensitivity composition not to be destroyed preferably; Have anti-oxidant and sterilization functions; Nontoxic, solvent-free remnants; Carbon dioxide is cheap and easy to get.
Technical problem to be solved by this invention is: a kind of method that removes remaining heavy metal in the rice is provided.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: removing the method for remaining heavy metal in the rice, is with the method for supercritical fluid as extractant.
In order to solve the problems of the technologies described above better, the further technical scheme that the present invention adopts is: describedly remove that the method for remaining heavy metal comprises static extracting and two stages of dynamic extraction in the rice.
In order to solve the problems of the technologies described above better, the further technical scheme that the present invention adopts is: described
Supercritical fluid is a supercritical carbon dioxide.
In order to solve the problems of the technologies described above better, the further technical scheme that the present invention adopts is: describedly remove that the method for remaining heavy metal may further comprise the steps in the rice: the rice that will contain heavy metal remnants is put into extraction kettle, extract as extractant with supercritical carbon dioxide, the temperature of extraction kettle and separating still is controlled at 20-50
oC, under the state of the carbon dioxide outlet valve of closing extraction kettle, carbon dioxide is injected extraction kettle, rise to 5-50MPa until the extraction kettle internal pressure, the carbon dioxide inlet valve of cutting out extraction kettle carries out static extracting, after 0-30 minutes, open the carbon dioxide inlet valve and the outlet valve of extraction kettle, make carbon dioxide flow through extraction kettle and carry out dynamic extraction, the temperature, pressure of dynamic extraction is identical with static extracting, the flow of carbon dioxide is per kilogram rice 0.5-20kg/h during dynamic extraction, and the time of dynamic extraction is 30-120 minutes, and carbon dioxide is cooled to 20-50 in separating still
oC is depressurized to 1-10Mpa, isolates the heavy metal composition that is extracted, and dynamic extraction is closed extraction kettle carbon dioxide inlet valve after finishing, and the pressure of extraction kettle is reduced to normal pressure, takes out through the rice grain after the extraction.
In order to solve the problems of the technologies described above better, the further technical scheme that the present invention adopts is: described extracting pressure is 10-20MPa, and extraction temperature is 35-45
oC, separating pressure are 1-5MPa, and separation temperature is 30-40
oC, the static extracting time is 10-20 minutes, and the dynamic extraction time is 45-90 minutes, and the flow of carbon dioxide is per kilogram rice 1-10kg/h during dynamic extraction.
Described heavy metal is lead, mercury, chromium, cadmium and arsenic.
Advantage of the present invention is: the present invention be with supercritical fluid as extractant effectively with heavy metal removing remaining in the rice.Pattern, nutritional labeling and the local flavor that can keep rice when removing heavy metal can not cause any secondary pollution to rice when removing heavy metal, can not produce environmentally harmful refuse yet.
The extraction process that the present invention adopts static extracting and dynamic extraction to combine has improved the removal efficiency of heavy metal greatly, makes to fail to detect heavy metal in the rice of extraction back.The static extracting stage: under the state that does not have carbon dioxide to flow, make the rice that contains heavy metal remnants in extraction kettle, fully contact a period of time with carbon dioxide earlier, carbon dioxide is fully infiltrated in the rice, heavy metal composition contained in the rice is dissolved in the CO 2 fluid.Behind static extracting, carry out dynamic extraction, promptly under the state that carbon dioxide flows, make rice fully contact a period of time with carbon dioxide, the heavy metal composition is dissolved in the carbon dioxide flows out extraction kettle with carbon dioxide, realization heavy metal composition separates with rice.The carbon dioxide that has dissolved the heavy metal composition has changed temperature and pressure in separating still, make heavy metal become and analyze, and realizes the regeneration of carbon dioxide, and the carbon dioxide after the regeneration is capable of circulation to be used for extraction.
The specific embodiment
Illustrate particular content of the present invention below.
Embodiment 1
The rice grain of leaded 0.071mg/kg, chromium 0.230mg/kg, cadmium 0.15 mg/kg is put into extraction kettle, the temperature of extraction kettle and separating still is controlled at 40 respectively
oC and 30
oC is closing the titanium dioxide of extraction kettle
Under the state of carbon outlet valve, carbon dioxide is injected extraction kettle, rise to 15MPa until the extraction kettle internal pressure, the carbon dioxide inlet valve of cutting out extraction kettle carries out static extracting, after 15 minutes, open the carbon dioxide inlet valve and the outlet valve of extraction kettle, make carbon dioxide flow through extraction kettle and carry out dynamic extraction, the temperature, pressure of dynamic extraction is identical with static extracting, the flow of carbon dioxide is per kilogram rice 7kg/h during dynamic extraction, the time of dynamic extraction is 45 minutes, and carbon dioxide is cooled to 25 in separating still
oC is depressurized to 5Mpa, and to isolate the heavy metal composition that is extracted, dynamic extraction is closed extraction kettle carbon dioxide inlet valve after finishing, and the pressure of extraction kettle is reduced to normal pressure, takes out the rice grain through extraction, and lead, chromium and cadmium all do not detect in the rice grain after the extraction.
Embodiment 2
The rice grain of leaded 0.190mg/kg, chromium 0.15mg/kg and arsenic 0.21mg/kg is put into extraction kettle, the temperature of extraction kettle and separating still is controlled at 45 respectively
oC and 25
oC, under the state of the carbon dioxide outlet valve of closing extraction kettle, carbon dioxide is injected extraction kettle, rise to 10MPa until the extraction kettle internal pressure, the carbon dioxide inlet valve of cutting out extraction kettle carries out static extracting, after 25 minutes, open the carbon dioxide inlet valve and the outlet valve of extraction kettle, make carbon dioxide flow through extraction kettle and carry out dynamic extraction, the temperature, pressure of dynamic extraction is identical with static extracting, the flow of carbon dioxide is per kilogram rice 3kg/h during dynamic extraction, and the time of dynamic extraction is 60 minutes, and carbon dioxide is cooled to 25 in separating still
oC is depressurized to 5Mpa, to isolate the heavy metal composition that is extracted, after dynamic extraction finishes, close extraction kettle carbon dioxide inlet valve, the pressure of extraction kettle is reduced to normal pressure, take out rice grain through extraction, in the rice grain after the extraction, lead content is less than 0.005mg/kg, and chromium content is less than 0.0001mg/kg, and arsenic content is less than 0.0005 mg/kg.
Embodiment 3
The rice grain of leaded 0.40mg/kg and chromium 0.11mg/kg is put into extraction kettle, the temperature of extraction kettle and separating still is controlled at 35 respectively
oC and 35
oC, under the state of the carbon dioxide outlet valve of closing extraction kettle, carbon dioxide is injected extraction kettle, rise to 20MPa until the extraction kettle internal pressure, the carbon dioxide inlet valve of cutting out extraction kettle carries out static extracting, after 10 minutes, open the carbon dioxide inlet valve and the outlet valve of extraction kettle, make carbon dioxide flow through extraction kettle and carry out dynamic extraction, the temperature, pressure of dynamic extraction is identical with static extracting, the flow of carbon dioxide is per kilogram rice 10kg/h during dynamic extraction, and the time of dynamic extraction is 30 minutes, and carbon dioxide is cooled to 15 in separating still
oC is depressurized to 4Mpa, and to isolate the heavy metal composition that is extracted, dynamic extraction is closed extraction kettle carbon dioxide inlet valve after finishing, and the pressure of extraction kettle is reduced to normal pressure, takes out the rice grain through extraction, does not detect lead in the rice grain after the extraction and does not also detect chromium.
Claims (6)
1. remove the method for remaining heavy metal in the rice, it is characterized in that, described method is with the method for supercritical fluid as extractant.
2. the method that removes remaining heavy metal in the rice according to claim 1 is characterized in that, described method comprises static extracting and two stages of dynamic extraction.
3. the method that removes remaining heavy metal in the rice according to claim 1 and 2 is characterized in that, described supercritical fluid is a supercritical carbon dioxide.
4. the method that removes remaining heavy metal in the rice according to claim 3, it is characterized in that, described method may further comprise the steps: the rice that will contain heavy metal remnants is put into extraction kettle, extract as extractant with supercritical carbon dioxide, the temperature of extraction kettle and separating still is controlled at 20-50
oC, under the state of the carbon dioxide outlet valve of closing extraction kettle, carbon dioxide is injected extraction kettle, rise to 5-50MPa until the extraction kettle internal pressure, the carbon dioxide inlet valve of cutting out extraction kettle carries out static extracting, after 0-30 minutes, open the carbon dioxide inlet valve and the outlet valve of extraction kettle, make carbon dioxide flow through extraction kettle and carry out dynamic extraction, the temperature, pressure of dynamic extraction is identical with static extracting, the flow of carbon dioxide is per kilogram rice 0.5-20kg/h during dynamic extraction, and the time of dynamic extraction is 30-120 minutes, and carbon dioxide is cooled to 20-50 in separating still
oC is depressurized to 1-10Mpa, isolates the heavy metal composition that is extracted, and dynamic extraction is closed extraction kettle carbon dioxide inlet valve after finishing, and the pressure of extraction kettle is reduced to normal pressure, takes out through the rice grain after the extraction.
5. the method that removes remaining heavy metal in the rice according to claim 4 is characterized in that, described extracting pressure is 10-20MPa, and extraction temperature is 35-45
oC, separating pressure are 1-5MPa, and separation temperature is 30-40
oC, the static extracting time is 10-20 minutes, and the dynamic extraction time is 45-90 minutes, and the flow of carbon dioxide is per kilogram rice 1-10kg/h during dynamic extraction.
6. the method that removes remaining heavy metal in the rice according to claim 5 is characterized in that, described heavy metal is lead, mercury, chromium, cadmium and arsenic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110050464XA CN102132799B (en) | 2011-03-03 | 2011-03-03 | Method for removing residual heavy metal in rice |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110050464XA CN102132799B (en) | 2011-03-03 | 2011-03-03 | Method for removing residual heavy metal in rice |
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| CN102132799A true CN102132799A (en) | 2011-07-27 |
| CN102132799B CN102132799B (en) | 2012-12-19 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230932A (en) * | 2013-04-11 | 2013-08-07 | 华北电力大学 | A device for remediation of organic contaminated soil by using supercritical CO2 fluid and a remediation method |
| CN103283931A (en) * | 2013-04-22 | 2013-09-11 | 义乌市海之纳生物工程有限公司 | Cadmium-eliminated desensitized rice protein, and preparation method and application thereof |
| CN103549234A (en) * | 2013-10-23 | 2014-02-05 | 华中农业大学 | Method of reducing heavy metals of cereals |
| CN104920966A (en) * | 2015-06-30 | 2015-09-23 | 中南林业科技大学 | Cadmium-removed rice flour and preparation method thereof |
| WO2018026734A1 (en) * | 2016-08-01 | 2018-02-08 | Shaklee Corporation | Removing heavy metals from rice |
| CN112661370A (en) * | 2020-12-30 | 2021-04-16 | 天津绿环农业种植有限公司 | Method for treating sludge by using organisms |
| CN115245191A (en) * | 2022-01-24 | 2022-10-28 | 王娜 | Cadmium removing method for rice |
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| KR20050058152A (en) * | 2003-12-11 | 2005-06-16 | 그린텍이십일 주식회사 | The Device & Method for Manufacturing Healthy Rice Using Subcritical/Supercritical Fluid and Supersonic Waves |
| CN101554211A (en) * | 2009-01-05 | 2009-10-14 | 王艺瑾 | Technique and industrial device for refining rice by supercritical polybasic fluid |
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2011
- 2011-03-03 CN CN201110050464XA patent/CN102132799B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050058152A (en) * | 2003-12-11 | 2005-06-16 | 그린텍이십일 주식회사 | The Device & Method for Manufacturing Healthy Rice Using Subcritical/Supercritical Fluid and Supersonic Waves |
| CN101554211A (en) * | 2009-01-05 | 2009-10-14 | 王艺瑾 | Technique and industrial device for refining rice by supercritical polybasic fluid |
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| 《理化检验－化学分册》 20011231 张艳君等 金属离子的超临界流体萃取技术的进展 1～6 第37卷, 第12期 * |
| 《生态环境》 20041231 牟仁祥等 水稻重金属污染研究进展 第417～419 1～6 第13卷, 第3期 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103230932A (en) * | 2013-04-11 | 2013-08-07 | 华北电力大学 | A device for remediation of organic contaminated soil by using supercritical CO2 fluid and a remediation method |
| CN103283931A (en) * | 2013-04-22 | 2013-09-11 | 义乌市海之纳生物工程有限公司 | Cadmium-eliminated desensitized rice protein, and preparation method and application thereof |
| CN103549234A (en) * | 2013-10-23 | 2014-02-05 | 华中农业大学 | Method of reducing heavy metals of cereals |
| CN104920966A (en) * | 2015-06-30 | 2015-09-23 | 中南林业科技大学 | Cadmium-removed rice flour and preparation method thereof |
| CN104920966B (en) * | 2015-06-30 | 2018-02-02 | 中南林业科技大学 | A kind of de- cadmium rice meal and preparation method thereof |
| WO2018026734A1 (en) * | 2016-08-01 | 2018-02-08 | Shaklee Corporation | Removing heavy metals from rice |
| CN112661370A (en) * | 2020-12-30 | 2021-04-16 | 天津绿环农业种植有限公司 | Method for treating sludge by using organisms |
| CN115245191A (en) * | 2022-01-24 | 2022-10-28 | 王娜 | Cadmium removing method for rice |
| CN115245191B (en) * | 2022-01-24 | 2023-11-14 | 王娜 | Cadmium removing method for rice |
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