CN106076301B - Preparation method of succinic anhydride modified shaddock peel oil absorption material - Google Patents
Preparation method of succinic anhydride modified shaddock peel oil absorption material Download PDFInfo
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- CN106076301B CN106076301B CN201610499376.0A CN201610499376A CN106076301B CN 106076301 B CN106076301 B CN 106076301B CN 201610499376 A CN201610499376 A CN 201610499376A CN 106076301 B CN106076301 B CN 106076301B
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- Prior art keywords
- shaddock peel
- succinic anhydride
- oil absorption
- peel oil
- preparation
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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
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method of acid anhydride modified shaddock peel oil absorption materials, which comprises the components of shaddock peel, succinic anhydride, an organic solvent and a catalyst, wherein the organic solvent can be or more of dimethyl sulfoxide, N-dimethylformamide, N-dimethyl benzamide, indoleacetic acid and the like, and the catalyst can be or more of pyridine, 4-dimethylamino pyridine, isoniazid, pyridine hydrochloride and the like.
Description
Technical Field
The invention relates to a preparation method of succinic anhydride modified shaddock peel oil absorption materials.
Background
The adsorption method is a commonly used method for treating water body oil pollution at present, a carrier of the adsorption method is mainly a porous adsorption material and mainly comprises an inorganic mineral material, a synthetic organic material and a natural organic material, the inorganic mineral material (such as clay, silicon dioxide, sepiolite and the like) is low in oil absorption capacity, poor in floatability and poor in water selection, extensive application of the inorganic mineral material in the environment is limited, the synthetic organic material (such as polyurethane) has high-efficiency oil absorption characteristics, but the synthetic technology is high in cost and operation cost, generates a large number of byproducts, is difficult to recover and degrade, and is easy to cause secondary pollution, kinds of adsorption materials are obtained, and the adsorption material which can be naturally degraded under natural conditions is a problem to be solved urgently at present.
The pomelo is which is a main fruit in China, is planted in regions in south, the pomelo peel accounts for about 50% of the total mass of the pomelo, is common agricultural and forestry wastes, contains a large amount of organic matters such as cellulose, hemicellulose, lignin and the like in the skin, and contains hydrophilic and oleophilic groups such as hydroxyl, carboxyl, ester and the like, compared with the traditional adsorbing material, the pomelo peel has the advantages of low price and general sources, is rich in a microporous structure, large in specific surface area, insoluble in water, easy to recover and treat, and the like, and has great potential in the aspect of water body oil pollution treatment.
Disclosure of Invention
The preparation method of anhydride modified shaddock peel oil absorption materials provided by the invention can be applied to adsorbing organic matters such as petroleum in water, and the like.
The specific technical scheme of the invention is as follows:
the preparation method of the anhydride modified shaddock peel oil absorption material is characterized by comprising the following preparation steps:
① pretreatment of shaddock peel:
naturally airing fresh and healthy shaddock peels, washing and soaking the shaddock peels by using deionized water, and drying the shaddock peels in a blast drying oven to constant weight. Removing the outer yellow skin, grinding, sieving, and placing in a dryer for use.
quantitative shaddock peel powder is weighed, 0.1mol/L NaOH solution is added, stirring is carried out for 2 hours at room temperature, suction filtration is carried out, absolute ethyl alcohol is used for washing, and drying is carried out at 60 ℃ until constant weight is achieved.
② modified shaddock peel:
and (3) taking a 100ml three-neck flask, sequentially adding the shaddock peel powder, the succinic anhydride, the organic solvent and the catalyst in the step ①, refluxing for 2h-6h at the temperature of 60-100 ℃, cooling, performing suction filtration, sequentially washing filter residues with absolute ethyl alcohol and deionized water, and transferring into a forced air drying oven to dry to constant weight at the temperature of 60 ℃ to obtain the modified shaddock peel oil absorption material.
The organic solvent in step ② may be one or more of dimethyl sulfoxide, N-dimethylformamide, N-dimethylbenzamide, indoleacetic acid, etc. .
The catalyst of step ② can be one or more of pyridine, 4-dimethylaminopyridine, isoniazid, pyridine hydrochloride, and the like.
The mass-to-volume ratio of the shaddock peel powder and the anhydride modifier in the step ② is preferably 1: 1-5.
The mass volume ratio of the shaddock peel powder and the organic solvent in the step ② is 1: 20-1: 100.
The invention has the beneficial effects that:
(1) the invention takes the shaddock peel as the raw material to prepare the oil absorption material, not only solves the problem of water body oil pollution treatment, but also can solve the problem of agricultural waste treatment, changes waste biomass into valuable, and has the double effects of purifying the environment.
(2) The surface layer of the shaddock peel adopted by the invention contains a large amount of cellulose, hemicellulose, lignin and the like, and the main functional groups have active groups such as-OH, -COOH, ester groups and the like, and simultaneously have hydrophilicity and lipophilicity, and can reduce the hydrophilicity and enhance the lipophilicity through chemical modification.
(3) The succinic anhydride modified shaddock peel oil absorption material prepared by the method has the advantages of strong operability, high adsorption capacity, strong oil-water selectivity, convenience in separation and high cycle number.
(4) The oil absorption material is prepared from the succinic anhydride modified shaddock peel, and the modifier belongs to a food additive, is non-toxic and harmless, and cannot cause secondary pollution.
Detailed Description
The present invention will be described in detail with reference to specific examples, but it should be understood that the present invention is not limited by the specific descriptions of the following examples.
Example
Taking fresh and healthy shaddock peel, naturally airing, washing and soaking with deionized water, and drying in a blast drying oven to constant weight. Removing the outer yellow skin, grinding, sieving, and placing in a dryer for use.
quantitative shaddock peel powder is weighed, 0.1mol/L NaOH solution is added, stirring is carried out for 2 hours at room temperature, suction filtration is carried out, absolute ethyl alcohol is used for washing, and drying is carried out at 60 ℃ until constant weight is achieved.
A100 ml three-necked flask was taken, and 1g of the above pretreated shaddock peel powder, 2g of succinic anhydride, 30ml of N, N-dimethylformamide and 0.3g of 4-dimethylaminopyridine were sequentially added thereto and refluxed at 80 ℃ for 3 hours. Cooling, performing suction filtration, washing filter residue with absolute ethyl alcohol and deionized water in sequence, and drying in a forced air drying oven at 60 ℃ to constant weight to obtain the modified shaddock peel oil absorption material.
Example two
Taking fresh and healthy shaddock peel, naturally airing, washing and soaking with deionized water, and drying in a blast drying oven to constant weight. Removing the outer yellow skin, grinding, sieving, and placing in a dryer for use.
quantitative shaddock peel powder is weighed, 0.1mol/L NaOH solution is added, stirring is carried out for 2 hours at room temperature, suction filtration is carried out, absolute ethyl alcohol is used for washing, and drying is carried out at 60 ℃ until constant weight is achieved.
A100 ml three-neck flask was taken, and 1g of the above pretreated shaddock peel powder, 1.5g of succinic anhydride, 30ml of dimethyl sulfoxide and 0.3g of isoniazid were sequentially added thereto, and refluxed at 100 ℃ for 2 hours. Cooling, performing suction filtration, washing filter residue with absolute ethyl alcohol and deionized water in sequence, and drying in a forced air drying oven at 60 ℃ to constant weight to obtain the modified shaddock peel oil absorption material.
Therefore, the above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent changes and modifications made in the content of the claims of the present invention should be considered as the technical scope of the present invention.
Claims (4)
- The preparation method of succinic anhydride modified shaddock peel oil absorption materials is used for adsorbing petroleum organic matters in a water body, and is characterized by comprising the following preparation steps:① pretreatment of shaddock peel:weighing quantitative above pericarpium Citri Grandis powder, adding 0.1mol/L NaOH solution, stirring at room temperature for 2 hr, vacuum filtering, washing with anhydrous ethanol, and oven drying at 60 deg.C to constant weight;② modified shaddock peel:and (2) taking a 100ml three-neck flask, sequentially adding the shaddock peel powder, the succinic anhydride, the organic solvent and the catalyst in the step ①, wherein the mass ratio of the shaddock peel powder to the succinic anhydride is 1: 1-5, refluxing for 2-6 h at 60-100 ℃, cooling, performing suction filtration, sequentially washing filter residues with absolute ethyl alcohol and deionized water, and transferring into a forced air drying oven to dry to constant weight at 60 ℃ to obtain the modified shaddock peel oil absorption material.
- 2. The method for preparing succinic anhydride-modified shaddock peel oil-absorbing materials according to claim 1, wherein the organic solvent used in step ② is or more selected from dimethylsulfoxide, N-dimethylformamide and N, N-dimethylbenzamide.
- 3. The method for preparing succinic anhydride modified shaddock peel oil absorption materials according to claim 1, wherein the catalyst in step ② is or more selected from pyridine, 4-dimethylaminopyridine, isoniazid and pyridine hydrochloride.
- 4. The preparation method of succinic anhydride modified shaddock peel oil absorption materials in claim 1, wherein the mass-to-volume ratio of the shaddock peel powder and the organic solvent in step ② is 1: 20-1: 100, the mass is in grams, and the volume is in milliliters.
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| CN201610499376.0A CN106076301B (en) | 2016-06-30 | 2016-06-30 | Preparation method of succinic anhydride modified shaddock peel oil absorption material |
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| CN201610499376.0A CN106076301B (en) | 2016-06-30 | 2016-06-30 | Preparation method of succinic anhydride modified shaddock peel oil absorption material |
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| CN106076301B true CN106076301B (en) | 2020-01-31 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107189245A (en) * | 2017-05-31 | 2017-09-22 | 晋源电气集团股份有限公司 | A kind of hot and humid environment power cable |
| CN107200942A (en) * | 2017-05-31 | 2017-09-26 | 晋源电气集团股份有限公司 | A kind of compound haloflex of high-temp resisting high-humidity resisting cable |
| CN110152611A (en) * | 2019-07-04 | 2019-08-23 | 浙江海洋大学 | A kind of preparation method of adsorbent material |
| CN115739035A (en) * | 2022-12-05 | 2023-03-07 | 南京信息工程大学 | Method for modifying kenaf straws by succinic anhydride |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863041A (en) * | 2012-09-17 | 2013-01-09 | 常州大学 | Method of removing oil in catering wastewater by adopting shaddock peel |
| CN104226269A (en) * | 2014-08-28 | 2014-12-24 | 天津市利顺塑料制品有限公司 | Modified shaddock peel adsorbent and preparation method thereof |
| CN104492386A (en) * | 2014-10-27 | 2015-04-08 | 河南城建学院 | Preparation method for oxalic-acid-modified pummelo pericarp biological adsorbent |
| CN104923168A (en) * | 2015-03-24 | 2015-09-23 | 信阳师范学院华锐学院 | Pomelo peel adsorbent modified with sulfo carbamates and preparation method of pomelo peel adsorbent |
| CN105289524A (en) * | 2015-11-09 | 2016-02-03 | 湖南有色金属研究院 | Shaddock peel heavy metal adsorbent and preparation method and application thereof |
-
2016
- 2016-06-30 CN CN201610499376.0A patent/CN106076301B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863041A (en) * | 2012-09-17 | 2013-01-09 | 常州大学 | Method of removing oil in catering wastewater by adopting shaddock peel |
| CN104226269A (en) * | 2014-08-28 | 2014-12-24 | 天津市利顺塑料制品有限公司 | Modified shaddock peel adsorbent and preparation method thereof |
| CN104492386A (en) * | 2014-10-27 | 2015-04-08 | 河南城建学院 | Preparation method for oxalic-acid-modified pummelo pericarp biological adsorbent |
| CN104923168A (en) * | 2015-03-24 | 2015-09-23 | 信阳师范学院华锐学院 | Pomelo peel adsorbent modified with sulfo carbamates and preparation method of pomelo peel adsorbent |
| CN105289524A (en) * | 2015-11-09 | 2016-02-03 | 湖南有色金属研究院 | Shaddock peel heavy metal adsorbent and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| Pomelo peel modified with acetic anhydride and styrene as new sorbents for removal of oil pollution;Wenbo Chai et al.;《Carbohydrate Polymers》;20150625;第132卷;第246页，2.1材料和2.2.1 AP的制备方法 * |
| 改性柚皮纤维素的制备及其对金属离子Cd2+的吸附研究;倪平;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20130215;第20,24页 * |
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