CN108097218A - A kind of preparation method for the rice hull adsorbent for being used to adsorb heavy metal ion - Google Patents
A kind of preparation method for the rice hull adsorbent for being used to adsorb heavy metal ion Download PDFInfo
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- CN108097218A CN108097218A CN201711366061.XA CN201711366061A CN108097218A CN 108097218 A CN108097218 A CN 108097218A CN 201711366061 A CN201711366061 A CN 201711366061A CN 108097218 A CN108097218 A CN 108097218A
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- Prior art keywords
- preparation
- metal ion
- heavy metal
- rice hull
- adsorb
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
Abstract
The present invention relates to a kind of for adsorbing the preparation method of the rice hull adsorbent of heavy metal ion, belong to adsorbent preparing technical field.The preparation method includes the following steps：1. being added to the water after rice husk is crushed, with acid for adjusting pH value to 5.5 6.2,70 80 DEG C of 0.5 1h of heating, filtering is washed to neutrality, dry；2. by step, 1. products obtained therefrom is added to the water, and adjusts pH value to 8.2 8.5,80 100 DEG C of 0.5 1h of heating with alkali, filtering is washed to neutrality, dry；3. by step, 2. 150 180 DEG C of 2 4h of reaction of products obtained therefrom and oxidant, filtering are washed, and activation obtains rice hull adsorbent.The present invention, which passes through, selects many condition of processing step and technological parameter, so as to get rice hull adsorbent there is excellent selectivity to heavy metal ion.
Description
Technical field
The present invention relates to a kind of for adsorbing the preparation method of the rice hull adsorbent of heavy metal ion, belongs to adsorbent preparation
Technical field.
Background technology
Rice husk is one layer of shell outside paddy, is commonly used for making soy sauce, wine and power generation, dressing up bag can also plant
Plant oyster mushroom.Several parts such as rice husk by meeting outside, inner glume, sterile lemma and rachilla form, the hair with temples hairy outside coetonium top.
Crude fibre (including lignin fibre and cellulose) and 20% pentose polymer (predominantly half fiber in rice husk containing about 40%
Dimension element).In addition, containing about the organic compounds such as 20% ash content and a small amount of crude protein, crude fat.
China is Rice Cropping country maximum in the world, according to the statistics of the Ministry of Agriculture, Chinese rice yield 18059 in 2005
Ten thousand tons, rice husk usually accounts for the 20% of paddy, calculates like this, more than 3,600 ten thousand tons of rice husk, rice husk resource very abundant.However, rice husk
Surface is hard, and silicone content is high, is not easy to be bacterially decomposed, and bulk density is small, discards welding, becomes the bag of meter Ye enterprises
Cloth-wrapper, the utilization of rice husk are significant.The main composition of rice husk is cellulose family, lignin and silicon class, kind and the place of production
Difference, difference, substantially composition are composition：Crude fibre 35.5-45% (polycondensation pentose 16-22%), lignin 21-
26%th, ash content 11.4-22%, silica 1 0-21%.According to the chemical composition of rice husk, its utilization can be divided into three categories：
Using its cellulose substances, such as furfural, xylose, levulic acid chemical products are produced using the method for hydrolysis；Utilize it
Silicon resource production such as sodium silicate, white carbon, silica silicon-containing compound；Using its carbon, protium, pass through pyrolysis
(gasification, burning etc.) obtains the energy.
Rice husk is made good use of and can not only reduce pollution, staticizes environment, and economic benefit can also be created, economize on resources, make
The good fortune mankind.There are many more the utilization ways and method of rice husk, such as rice husk processing activated carbon, battery graphite Carbon Materials, rice husk
Plate etc..
The production technology of existing activated carbon is：Rice husk is added into 8% soda ash after high-temperature retorting is carried out in closed iron container, is added
Same amount boiling, be washed till with cold water neutrality, heating, drying, removal of impurities, crushing, sieving (100 mesh) efficient fining agent activated carbon.
The content of the invention
The present invention has obtained having excellent selection to heavy metal ion by the improvement to rice husk base adsorbent preparation process
The rice husk base adsorbent of property.
The present invention provides a kind of for adsorbing the preparation method of the rice hull adsorbent of heavy metal ion, the preparation method
Include the following steps：
1. it is added to the water after rice husk is crushed, with acid for adjusting pH value to 5.5-6.2,70-80 DEG C of heating 0.5-1h, mistake
Filter is washed to neutrality, dry；
2. by step, 1. products obtained therefrom is added to the water, and pH value is adjusted to 8.2-8.5,80-100 DEG C of heating 0.5- with alkali
1h, filtering are washed to neutrality, dry；
3. by step, 2. 150-180 DEG C of reaction 2-4h of products obtained therefrom and oxidant, filtering are washed, and activation obtains rice husk suction
Attached dose.
The granularity of rice husk is preferably 200-300 mesh after crushing of the present invention.
1. the weight ratio of middle rice husk and water is preferably 1 to step of the present invention：15-30.
1. the weight ratio of middle rice husk and water is more preferably 1 to step of the present invention：18-25.
2. 1. the weight ratio of products obtained therefrom and water is preferably 1 to middle step to step of the present invention：5-12.
2. 1. the weight ratio of products obtained therefrom and water is more preferably 1 to middle step to step of the present invention：6-10.
Oxidant of the present invention is preferably sulfuric acid and nitric acid.
The mass fraction of sulfuric acid of the present invention is preferably 30-50%.
The mass fraction of sulfuric acid of the present invention is more preferably 35-45%.
The mass fraction of nitric acid of the present invention is preferably 20-30%.
The mass fraction of nitric acid of the present invention is more preferably 22-28%.
The weight ratio of sulfuric acid and nitric acid of the present invention is preferably 1：1-5.
The weight ratio of sulfuric acid and nitric acid of the present invention is more preferably 1：1.5-3.
2. the weight ratio of products obtained therefrom and oxidant is preferably 1 to step of the present invention：5-10.
2. the weight ratio of products obtained therefrom and oxidant is more preferably 1 to step of the present invention：5.5-8.
The method of activation of the present invention is preferably：600-750 DEG C of activation 1-3h.
Preparation method of the present invention includes the following steps：1. being added to the water after rice husk is crushed, acid for adjusting pH value is used
To 5.5-6.2,70-80 DEG C of heating 0.5-1h, filtering is washed to neutrality, dry；2. by step, 1. products obtained therefrom is added to water
In, pH value is adjusted to 8.2-8.5 with alkali, and 80-100 DEG C of heating 0.5-1h, filtering is washed to neutrality, dry；3. by step 2. institute
150-180 DEG C of reaction 2-4h of product and oxidant is obtained, filters, washs, activate, obtain rice hull adsorbent.The present invention passes through to work
The many condition of skill step and technological parameter select, so as to get rice hull adsorbent to heavy metal ion have excellent selectivity,
Solve the problems, such as that existing rice hull adsorbent counterweight metalloform-selective is poor.
Specific embodiment
Following non-limiting examples can make those of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Embodiment 1
A kind of preparation method for the rice hull adsorbent for being used to adsorb heavy metal ion, the preparation method include following step
Suddenly：
1. being added to the water after rice husk is crushed to 200-300 mesh, pH value is adjusted to 6.0,80 DEG C of heating with dilute hydrochloric acid
0.5h, filtering are washed to neutrality, dry；
1. the weight ratio of middle rice husk and water is 1 to step：30；
2. by step, 1. products obtained therefrom is added to the water, and pH value is adjusted to 8.3,90 DEG C of heating with sodium hydroxide solution
0.5h, filtering are washed to neutrality, dry；
2. 1. the weight ratio of products obtained therefrom and water is 1 to middle step to step：12；
3. by step, 2. 175 DEG C of reaction 2.5h of products obtained therefrom and oxidant, filtering, washing, 700 DEG C of activation 2h obtain rice
Shell adsorbent；
Oxidant is：The weight of the nitric acid that the sulfuric acid that mass fraction is 50% is 20% with mass fraction, sulfuric acid and nitric acid
Than for 1：3；
2. the weight ratio of products obtained therefrom and oxidant is 1 to step：9.
Embodiment 2
A kind of preparation method for the rice hull adsorbent for being used to adsorb heavy metal ion, the preparation method include following step
Suddenly：
1. being added to the water after rice husk is crushed to 200-300 mesh, pH value is adjusted to 5.8,75 DEG C of heating with dilute hydrochloric acid
0.5h, filtering are washed to neutrality, dry；
1. the weight ratio of middle rice husk and water is 1 to step：25；
2. by step, 1. products obtained therefrom is added to the water, and pH value is adjusted to 8.5,100 DEG C of heating with sodium hydroxide solution
0.5h, filtering are washed to neutrality, dry；
2. 1. the weight ratio of products obtained therefrom and water is 1 to middle step to step：8；
3. by step, 2. 160 DEG C of reaction 3h of products obtained therefrom and oxidant, filtering, washing, 650 DEG C of activation 3h obtain rice husk
Adsorbent；
Oxidant is：The weight of the nitric acid that the sulfuric acid that mass fraction is 40% is 25% with mass fraction, sulfuric acid and nitric acid
Than for 1：2；
2. the weight ratio of products obtained therefrom and oxidant is 1 to step：7.
Embodiment 3
A kind of preparation method for the rice hull adsorbent for being used to adsorb heavy metal ion, the preparation method include following step
Suddenly：
1. be added to the water after rice husk is crushed to 200-300 mesh, with dilute hydrochloric acid adjust pH value to 6.2,70 DEG C heating 1h,
Filtering is washed to neutrality, dry；
1. the weight ratio of middle rice husk and water is 1 to step：20；
2. by step, 1. products obtained therefrom is added to the water, with sodium hydroxide solution adjust pH value to 8.2,85 DEG C heating 1h,
Filtering is washed to neutrality, dry；
2. 1. the weight ratio of products obtained therefrom and water is 1 to middle step to step：5；
3. by step, 2. 180 DEG C of reaction 2h of products obtained therefrom and oxidant, filtering, washing, 750 DEG C of activation 1h obtain rice husk
Adsorbent；
Oxidant is：The weight of the nitric acid that the sulfuric acid that mass fraction is 35% is 28% with mass fraction, sulfuric acid and nitric acid
Than for 1：1.5.
2. the weight ratio of products obtained therefrom and oxidant is 1 to step：5.5.
Test case 1
Rice hull adsorbent prepared by embodiment 1-3 is used to adsorb Pb2+, test adsorbance be respectively 172mg/g,
178mg/g、175mg/g。
Claims (10)
1. a kind of preparation method for the rice hull adsorbent for being used to adsorb heavy metal ion, it is characterised in that：The preparation method bag
Include following steps：
1. being added to the water after rice husk is crushed, with acid for adjusting pH value to 5.5-6.2,70-80 DEG C of heating 0.5-1h, filtering is washed
It washs to neutrality, it is dry；
2. by step, 1. products obtained therefrom is added to the water, and pH value is adjusted to 8.2-8.5,80-100 DEG C of heating 0.5-1h, mistake with alkali
Filter is washed to neutrality, dry；
3. by step, 2. 150-180 DEG C of reaction 2-4h of products obtained therefrom and oxidant, filtering are washed, and activation obtains rice husk absorption
Agent.
2. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 1, it is characterised in that：Institute
The granularity for stating rice husk after crushing is 200-300 mesh.
3. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 2, it is characterised in that：Institute
Stating step, 1. the weight ratio of middle rice husk and water is 1：15-30.
4. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 3, it is characterised in that：Institute
Stating step, 2. 1. the weight ratio of products obtained therefrom and water is 1 to middle step：5-12.
5. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 4, it is characterised in that：Institute
Oxidant is stated as sulfuric acid and nitric acid.
6. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 5, it is characterised in that：Institute
The mass fraction for stating sulfuric acid is 30-50%.
7. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 6, it is characterised in that：Institute
The mass fraction for stating nitric acid is 20-30%.
8. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 7, it is characterised in that：Institute
The weight ratio for stating sulfuric acid and nitric acid is 1：1-5.
9. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 8, it is characterised in that：Institute
Stating step, 2. the weight ratio of products obtained therefrom and oxidant is 1：5-10.
10. it is used to adsorb the preparation method of the rice hull adsorbent of heavy metal ion according to claim 9, it is characterised in that：
The method of the activation is：600-750 DEG C of activation 1-3h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711366061.XA CN108097218A (en) | 2017-12-18 | 2017-12-18 | A kind of preparation method for the rice hull adsorbent for being used to adsorb heavy metal ion |
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| CN201711366061.XA CN108097218A (en) | 2017-12-18 | 2017-12-18 | A kind of preparation method for the rice hull adsorbent for being used to adsorb heavy metal ion |
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| CN108097218A true CN108097218A (en) | 2018-06-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111569838A (en) * | 2020-04-29 | 2020-08-25 | 嘉兴学院 | Adsorbent for adsorbing heavy metal ions and preparation method thereof |
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- 2017-12-18 CN CN201711366061.XA patent/CN108097218A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111569838A (en) * | 2020-04-29 | 2020-08-25 | 嘉兴学院 | Adsorbent for adsorbing heavy metal ions and preparation method thereof |
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Application publication date: 20180601 |