CN111215025A - Composite adsorbent and preparation method and application thereof - Google Patents
Composite adsorbent and preparation method and application thereof Download PDFInfo
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- CN111215025A CN111215025A CN201911228276.4A CN201911228276A CN111215025A CN 111215025 A CN111215025 A CN 111215025A CN 201911228276 A CN201911228276 A CN 201911228276A CN 111215025 A CN111215025 A CN 111215025A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a composite adsorbent and a preparation method and application thereof, wherein the composite adsorbent comprises the following components in parts by mass: 40-66.6 parts of alumina, 33.3-60 parts of clay and 0.1-5 parts of lanthanum hydroxide; the preparation method of the composite adsorbent comprises the following steps: (1) preparing raw materials, adding alumina, argil and lanthanum hydroxide into a solvent to obtain a mixed solution; (2) and controlling the pH value of the mixed solution to be 7.5-8.5, and filtering after complete reaction to obtain filter residue, namely the composite adsorbent. The composite adsorbent can be applied to impurity removal and adsorption processes of the plant insulating oil, has the advantages of strong adsorption capacity and stable chemical property, and can remarkably reduce the acid value and the dielectric loss factor of the plant insulating oil.
Description
Technical Field
The invention relates to the field of grease processing, in particular to a composite adsorbent and a preparation method and application thereof.
Background
Mineral insulating oil is widely adopted in oil-immersed power transformers, and the effects of insulation, heat dissipation, cooling, arc extinguishing and the like can be achieved. However, due to the defects of low safety, poor degradability, non-regeneration and the like of the mineral insulating oil, the development of a novel liquid insulating medium becomes a research hotspot and has a good development prospect. The vegetable insulating oil is prepared by natural oil crops through processes of squeezing or leaching, refining and the like, has good physical, chemical and electrical insulating properties, can meet the requirements of oil for electric power, has a burning point higher than 300 ℃, has outstanding fireproof safety performance, has a natural biodegradation rate of more than 97 percent, and cannot cause environmental pollution to soil, water sources and the like; the raw material source is wide, the renewable advantage is achieved, and the liquid insulating material can be used as a novel liquid insulating material for replacing mineral insulating oil.
In the production process of the vegetable insulating oil, methods such as an alkali refining method, an acid clay adsorption refining method, an activated alumina method and the like are usually adopted to reduce the acid value and the dielectric loss factor of the vegetable oil, but the methods have the disadvantages of complex process, large adsorbent dosage and poor effect, and are difficult to meet the index requirements of the vegetable insulating oil on the acid value and the dielectric loss factor.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a composite adsorbent and a preparation method and application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the composite adsorbent comprises the following components in parts by mass: 40-66.6 parts of alumina, 33.3-60 parts of clay and 0.1-5 parts of lanthanum hydroxide. The composite adsorbent is composed of the alumina, the argil and the lanthanum hydroxide, so that the adsorption effect of the composite adsorbent on impurities can be improved, and the adsorption capacity of the composite adsorbent on complex components can be improved by utilizing the difference of the sizes of pores of different substances; in addition, the strong acid value adsorption performance of the aluminum oxide and the lanthanum hydroxide can greatly improve the acid value reduction capability of the composite adsorbent to an adsorbed system, thereby improving the application effect of the composite adsorbent in vegetable oil adsorption impurity removal.
Preferably, in the above aspect, the alumina is basic alumina. The alkalinity of the alkaline alumina is stronger than that of the alumina, and the effect of the composite adsorbent of the technical scheme on reducing the acid value can be obviously enhanced.
Preferably, the pH of the suspension of basic alumina is 10.
Preferably, the alumina has a particle size of 100 to 200 mesh. The limitation on the particle size of the alumina is one of the key factors influencing the adsorption effect of the composite adsorbent, the small particle size of the alumina causes the small particle size of the whole composite adsorbent, the composite adsorbent is not easy to separate from an adsorbed object such as insulating oil, and the large particle size reduces the adsorption effect of the composite adsorbent.
Preferably, in the above aspect, the clay is activated bentonite. The clay is activated to improve the specific surface area of the clay, remove non-silicon compounds in the clay and improve the interlayer cation exchange capacity, thereby improving the adsorption capacity of the composite adsorbent.
Preferably, the activation treatment is performed by: and soaking the bentonite in dilute sulfuric acid with the mass fraction of 8% -15%, and then rinsing until the pH of a rinsing solution is 3.8-4.0 to obtain the argil.
Preferably, the particle size of the composite adsorbent is 400-600 nm. If the particle size of the composite adsorbent is too small, the composite adsorbent is not easily separated from an adsorbate such as insulating oil, and if the particle size of the composite adsorbent is too large, the adsorption effect of the composite adsorbent is reduced, and the adsorption effect and the separation difficulty of the composite adsorbent can be balanced by selecting the proper particle size of the composite adsorbent.
Based on the same technical concept, the invention also provides a preparation method of the composite adsorbent, which comprises the following steps:
(1) preparing raw materials, adding alumina, argil and lanthanum hydroxide into a solvent to obtain a mixed solution;
(2) and controlling the pH value of the mixed solution to be 7.5-8.5, and filtering after complete reaction to obtain filter residue, namely the composite adsorbent.
The method is simple to operate, all components of the prepared composite adsorbent are uniformly mixed, the particle size distribution of the composite adsorbent is relatively uniform, and the adsorption performance of the composite adsorbent can be ensured.
Preferably, in the step (2), the pH of the mixed solution is controlled by adding an aqueous ammonia solution to the mixed solution. The raw material is easy to obtain by using ammonia water to adjust the pH, and impurity ions can not be introduced into the composite adsorbent system.
Based on the same technical concept, the invention also provides application of the composite adsorbent, and the composite adsorbent can be applied to impurity removal and adsorption processes of the vegetable insulating oil.
Compared with the prior art, the invention has the advantages that:
(1) the composite adsorbent provided by the invention has strong adsorption capacity on the vegetable oil insulating oil and stable chemical property, is simple to use and simple and convenient to operate when being applied to impurity removal and adsorption processes of the vegetable oil insulating oil, can obviously reduce the acid value of the vegetable oil insulating oil, can enable the acid value to be lower than 0.03mgKOH/g, can also obviously reduce the dielectric loss factor of the vegetable oil insulating oil, and can enable the dielectric loss factor to be lower than 0.03.
(2) The preparation method has simple process, and the prepared composite adsorbent has the advantages of uniform mixing of all components and uniform particle size distribution.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
The adsorbent of the embodiment comprises the following components in parts by mass: 50 parts of alkaline alumina, 50 parts of argil and 1 part of lanthanum hydroxide; wherein the particle size of the alkaline alumina is 100 meshes, and the pH of the suspension of the alkaline alumina is 10; the argil is bentonite subjected to activation treatment, and the specific activation operation is as follows: the bentonite is dipped in dilute sulphuric acid with the mass fraction of 8 percent for activation treatment, and then rinsed by water until the pH value of the washing liquid is 3.8, and dried at 150 ℃ to obtain the argil.
The preparation method of the adsorbent of the embodiment comprises the following steps:
(1) adding 100 g of alkaline alumina, 100 g of activated clay and 2 g of lanthanum hydroxide into an aqueous solution to obtain a mixed solution;
(2) and adjusting the pH value of the mixed solution to 8.0 by using ammonia water, filtering after complete precipitation, and drying filter residues at 150 ℃ to obtain the adsorbent.
1 kg of vegetable oil which is washed with alkali, decolored and dehydrated is taken, 3 w% of the adsorbent of the embodiment is added, the mixture is stirred for 0.5 hour at the temperature of 45 ℃ and then is kept stand, and clear liquid is taken to measure the acid value and the dielectric loss factor of the vegetable oil, and the measuring method is shown in the oil quality standard of soybean plant transformers (DL// T1360 2014).
The acid value and the dielectric loss tangent before the adsorption treatment were 0.125mgKOH/g and 0.938, respectively, and the acid value and the dielectric loss tangent after the treatment were 0.027mgKOH/g and 0.0234, respectively.
Example 2
The adsorbent of the embodiment comprises the following components in parts by mass: 50 parts of alkaline alumina, 60 parts of argil and 1.25 parts of lanthanum hydroxide; wherein the particle size of the alkaline alumina is 200 meshes, and the pH of the suspension of the alkaline alumina is 10; the argil is bentonite subjected to activation treatment, and the specific activation operation is as follows: the bentonite is soaked in dilute sulfuric acid with the mass fraction of 15% for activation treatment, rinsed by water until the pH value of a washing liquid is 4, and dried at 180 ℃ to obtain the argil.
The preparation method of the adsorbent of the embodiment comprises the following steps:
(1) adding 100 g of alkaline alumina, 120 g of activated clay and 2.5 g of lanthanum hydroxide into an aqueous solution to obtain a mixed solution;
(2) and adjusting the pH value of the mixed solution to 8.2 by using ammonia water, filtering after complete precipitation, and drying filter residues at 150 ℃ to obtain the adsorbent.
1 kg of vegetable oil which is washed with alkali, decolored and dehydrated is taken, 3.5 w% of the adsorbent of the embodiment is added, the mixture is stirred for 0.5 hour at the temperature of 45 ℃ and then is kept stand, and clear liquid is taken to measure the acid value and the dielectric loss factor of the vegetable oil, wherein the measuring method is shown in the oil quality standard of soybean plant transformers (DL// T1360-2014).
The acid value and the dielectric loss tangent before the adsorption treatment were 0.137mgKOH/g and 0.852, respectively, and the acid value and the dielectric loss tangent after the treatment were 0.029mgKOH/g and 0.0215, respectively.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-described embodiments. Modifications and variations that may occur to those skilled in the art without departing from the spirit and scope of the invention are to be considered as within the scope of the invention.
Claims (10)
1. The composite adsorbent is characterized by comprising the following components in parts by mass: 40-66.6 parts of alumina, 33.3-60 parts of clay and 0.1-5 parts of lanthanum hydroxide.
2. The composite adsorbent of claim 1, wherein the alumina is basic alumina.
3. The composite adsorbent of claim 2, wherein said suspension of basic alumina has a pH of 10.
4. The composite adsorbent of claim 1, wherein the alumina has a particle size of 100 to 200 mesh.
5. The composite adsorbent of claim 1, wherein said clay is activated bentonite.
6. The composite adsorbent of claim 5, wherein the activation treatment is specifically operative to: and soaking the bentonite in dilute sulfuric acid with the mass fraction of 8% -15%, and then rinsing with distilled water until the pH of a rinsing solution is 3.8-4.0 to obtain the argil.
7. The composite adsorbent according to any one of claims 1 to 6, wherein the composite adsorbent has a particle size of 400 to 600 nm.
8. A preparation method of the composite adsorbent as claimed in any one of claims 1 to 7, characterized by comprising the following steps:
(1) preparing raw materials, adding alumina, argil and lanthanum hydroxide into a solvent to obtain a mixed solution;
(2) and adjusting the pH value of the mixed solution to 7.5-8.5, and filtering after complete reaction to obtain filter residue, namely the composite adsorbent.
9. The method of claim 8, wherein the pH of the mixed solution is controlled by adding an aqueous ammonia solution to the mixed solution in the step (2).
10. The application of the composite adsorbent according to claims 1-7, wherein the composite adsorbent is applied to impurity removal and adsorption processes of vegetable insulating oil.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111760547A (en) * | 2020-07-08 | 2020-10-13 | 山东西奥生物科技有限公司 | Deep treatment process for natural ester insulating oil, super-hydrophilic adsorbent, preparation method and application thereof |
CN116731773A (en) * | 2023-06-13 | 2023-09-12 | 上海江天高分子材料有限公司 | Degradable soybean-based natural ester insulating oil and preparation method and application thereof |
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CN1068049A (en) * | 1991-06-27 | 1993-01-20 | 吴凤义 | Purifying agent for insulating oil |
CN101462733A (en) * | 2009-01-13 | 2009-06-24 | 安徽膨润矿业科技有限公司 | Active clay and preparation thereof |
CN104232302A (en) * | 2014-10-09 | 2014-12-24 | 重庆大学 | Vegetable insulating oil treating full-set process |
CN108913351A (en) * | 2018-04-20 | 2018-11-30 | 国网湖北省电力有限公司孝感供电公司 | A kind of method of novel plant insulating oil deacidification value |
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2019
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CN104232302A (en) * | 2014-10-09 | 2014-12-24 | 重庆大学 | Vegetable insulating oil treating full-set process |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111760547A (en) * | 2020-07-08 | 2020-10-13 | 山东西奥生物科技有限公司 | Deep treatment process for natural ester insulating oil, super-hydrophilic adsorbent, preparation method and application thereof |
CN111760547B (en) * | 2020-07-08 | 2023-05-09 | 山东西奥生物科技有限公司 | Deep treatment process of natural ester insulating oil, super-hydrophilic adsorbent, and preparation method and application thereof |
CN116731773A (en) * | 2023-06-13 | 2023-09-12 | 上海江天高分子材料有限公司 | Degradable soybean-based natural ester insulating oil and preparation method and application thereof |
CN116731773B (en) * | 2023-06-13 | 2023-12-12 | 上海江天高分子材料有限公司 | Degradable soybean-based natural ester insulating oil and preparation method and application thereof |
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