CN114100587A - Large-scale production method of chitosan adsorbent for regeneration of deteriorated insulating oil - Google Patents
Large-scale production method of chitosan adsorbent for regeneration of deteriorated insulating oil Download PDFInfo
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- CN114100587A CN114100587A CN202111490461.8A CN202111490461A CN114100587A CN 114100587 A CN114100587 A CN 114100587A CN 202111490461 A CN202111490461 A CN 202111490461A CN 114100587 A CN114100587 A CN 114100587A
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 80
- 239000003463 adsorbent Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000011031 large-scale manufacturing process Methods 0.000 title claims abstract description 19
- 230000008929 regeneration Effects 0.000 title abstract description 16
- 238000011069 regeneration method Methods 0.000 title abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 15
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000032683 aging Effects 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 230000001172 regenerating effect Effects 0.000 claims description 8
- 239000004677 Nylon Substances 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 238000004806 packaging method and process Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 12
- 239000003921 oil Substances 0.000 description 52
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000843 powder Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 239000002920 hazardous waste Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
- C10M175/0008—Working-up used lubricants to recover useful products ; Cleaning with the use of adsorbentia
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a large-scale production method of a chitosan adsorbent for regeneration of deteriorated insulating oil, which comprises the following steps: (1) adding silicon-aluminum gel into chitosan gel liquid, stirring for 0.5h, and slowly dripping NaOH solution with the concentration of 2mol/L under the stirring state to obtain mixed liquid; wherein the mass volume ratio (g/ml) of the silicon-aluminum gel to the chitosan gel liquid is 9:100, and the volume ratio of the NaOH solution to the chitosan gel liquid is 1-10: 100; (2) stirring the mixed solution in a constant temperature water bath at 70 ℃ for 2h to slowly mineralize chitosan on the surface of the XDK to form chitosan gel, adjusting the chitosan gel to be neutral, aging for 24h, and drying to obtain the chitosan adsorbent XDK-CSK. The invention has simple production process, easy control of the process and low production cost, realizes the large-scale production of the chitosan adsorbent, and the prepared chitosan adsorbent has excellent adsorption regeneration treatment effect on the deteriorated insulating oil and strong market competitiveness.
Description
Technical Field
The invention belongs to the technical field of deteriorated insulating oil regeneration, and particularly relates to a large-scale production method of a chitosan adsorbent for deteriorated insulating oil regeneration.
Background
Deteriorated insulating oil can become a "hazardous waste" defined by national environmental regulations. Such "hazardous waste" not only causes great resource waste and economic loss, but also causes serious harm to human life safety and ecological environment, etc. However, the existing domestic and foreign restoration method for the deteriorated insulating oil has the problems of secondary pollution, low restoration speed, complex process, low efficiency and the like, and the performance restoration for the deteriorated insulating oil has the problems of single method, poor effect, environmental pollution and the like.
Most of the components in the deteriorated insulating oil are recyclable, and it is preferable to perform adsorption regeneration treatment. The adsorbent is used to regenerate deteriorated insulating oil, and the degraded oil, which is harmful to its physical and chemical properties, is deeply adsorbed by means of molecular adsorption, so that the oil product is regenerated and refined, and the deteriorated oil can reach the use standard again. However, the existing adsorbent has poor adsorption regeneration treatment effect on the deteriorated insulating oil, or has good adsorption regeneration treatment effect on the deteriorated insulating oil, but the production process is complex, the process is not easy to control, the production cost is high, and large-scale production cannot be realized.
Therefore, a large-scale production method of the adsorbent with excellent adsorption regeneration treatment effect on the deteriorated insulating oil is researched and designed, and the method has important economic significance, environmental protection significance and engineering application value for realizing power operation and maintenance safety, economic production, environmental protection and the like.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides a large-scale production method of a chitosan adsorbent for regenerating deteriorated insulating oil, which has the advantages of simple production process, easily controlled process, low production cost and realization of large-scale production, and the prepared chitosan adsorbent has excellent adsorption regeneration treatment effect on the deteriorated insulating oil.
The technical scheme for solving the technical problems is as follows:
a large-scale production method of a chitosan adsorbent for regenerating deteriorated insulating oil comprises the following steps:
(1) adding silicon-aluminum gel into chitosan gel liquid, stirring for 0.5h, and slowly dripping NaOH solution with the concentration of 2mol/L under the stirring state to obtain mixed liquid;
wherein the mass volume ratio (g/ml) of the silicon-aluminum gel to the chitosan gel liquid is 9:100, and the volume ratio of the NaOH solution to the chitosan gel liquid is 1-10: 100;
(2) stirring the mixed solution in a constant temperature water bath at 70 ℃ for 2h to slowly mineralize chitosan on the surface of the XDK to form chitosan gel, adjusting the chitosan gel to be neutral, aging for 24h, and drying to obtain the chitosan adsorbent XDK-CSK.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in the step (2), the drying time is 24-48h, and the temperature is 85-95 ℃.
Further, in the step (2), the chitosan adsorbent XDK-CSK obtained after drying is packaged by a nylon cloth packaging bag with the length of 10cm and the width of 5 cm.
Further, the package specification of the chitosan adsorbent XDK-CSK is 100-500 g/bag.
The invention has the beneficial effects that: the invention has simple production process, easy control of the process and low production cost, realizes the large-scale production of the chitosan adsorbent, and the prepared chitosan adsorbent has excellent adsorption regeneration treatment effect on the deteriorated insulating oil and strong market competitiveness.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Unless otherwise indicated, the raw materials and equipment used in the present invention are conventional in the art (conventional commercial products) and are commercially available.
Example 1
The large-scale production method of the chitosan adsorbent for regenerating the deteriorated insulating oil, which is designed by the embodiment, comprises the following steps of:
(1) taking 10L of chitosan gel liquid, adding 900g of silicon-aluminum gel, stirring for 0.5h, and slowly dripping 100ml of NaOH solution with the concentration of 2mol/L under the stirring state to obtain a mixed solution;
(2) stirring the mixed solution in a constant temperature water bath at 70 ℃ for 2h to slowly mineralize chitosan on the surface of the XDK to form chitosan gel, adjusting the chitosan gel to be neutral, aging for 24h, and drying to obtain the chitosan adsorbent XDK-CSK.
50kg of deteriorated insulating oil to be treated was poured into an oil storage tank, 1kg of the chitosan adsorbent XDK-CSK prepared in this example was cut and loaded into an adsorption tank, the deteriorated insulating oil was adsorbed at a flow rate of 100L/min at 60 ℃ for 24 hours in a sealed circulation manner, and then the insulating oil in the filtration system was discharged.
Example 2
The large-scale production method of the chitosan adsorbent for regenerating the deteriorated insulating oil, which is designed by the embodiment, comprises the following steps of:
(1) taking 10L of chitosan gel liquid, adding 900g of silicon-aluminum gel, stirring for 0.5h, and slowly dripping 300ml of NaOH solution with the concentration of 2mol/L under the stirring state to obtain a mixed solution;
(2) stirring the mixed solution in a constant temperature water bath at 70 ℃ for 2h to slowly mineralize chitosan on the surface of the XDK to form chitosan gel, adjusting the chitosan gel to be neutral, aging for 24h, and drying at 90 ℃ for 36h to obtain the chitosan adsorbent XDK-CSK.
50kg of deteriorated insulating oil to be treated was poured into an oil storage tank, 1.5kg of the chitosan adsorbent XDK-CSK prepared in this example was cut and placed in an adsorption tank, the deteriorated insulating oil was adsorbed at a flow rate of 150L/min under a sealed circulation at 25 ℃ for 18 hours, and then the insulating oil in the filtration system was discharged.
Example 3
The large-scale production method of the chitosan adsorbent for regenerating the deteriorated insulating oil, which is designed by the embodiment, comprises the following steps of:
(1) taking 10L of chitosan gel liquid, adding 900g of silicon-aluminum gel, stirring for 0.5h, and slowly dripping 1000ml of NaOH solution with the concentration of 2mol/L under the stirring state to obtain a mixed solution;
(2) stirring the mixed solution in a constant-temperature water bath at 70 ℃ for 2h to slowly mineralize chitosan on the surface of the XDK to form chitosan gel, adjusting the chitosan gel to be neutral, aging for 24h, and drying at 85 ℃ for 48h to obtain the chitosan adsorbent XDK-CSK.
50kg of deteriorated insulating oil to be treated was poured into an oil storage tank, 1.5kg of the chitosan adsorbent XDK-CSK prepared in this example was cut and placed in an adsorption tank, the deteriorated insulating oil was adsorbed at a flow rate of 120L/min under a sealed circulation at 35 ℃ for 12 hours, and then the insulating oil in the filtration system was discharged.
Example 4
The large-scale production method of the chitosan adsorbent for regenerating the deteriorated insulating oil, which is designed by the embodiment, comprises the following steps of:
(1) taking 10L of chitosan gel liquid, adding 900g of silicon-aluminum gel, stirring for 0.5h, and slowly dripping 600ml of NaOH solution with the concentration of 2mol/L under the stirring state to obtain a mixed solution;
(2) stirring the mixed solution in a constant temperature water bath at 70 ℃ for 2h to slowly mineralize chitosan on the surface of the XDK to form chitosan gel, adjusting the chitosan gel to be neutral, aging for 24h, and drying at 95 ℃ for 24h to obtain the chitosan adsorbent XDK-CSK.
50kg of deteriorated insulating oil to be treated was poured into an oil storage tank, 2kg of the chitosan adsorbent XDK-CSK prepared in this example was cut and loaded into an adsorption tank, the deteriorated insulating oil was adsorbed at a flow rate of 140L/min at 45 ℃ for 6 hours in a sealed cycle, and then the insulating oil in the filtration system was discharged.
Comparative example 1
The large-scale production method of the chitosan adsorbent for regenerating the deteriorated insulating oil, which is designed by the comparative example, comprises the following steps:
(1) taking 10L of chitosan gel liquid, adding 800g of silicon-aluminum gel, stirring for 0.5h, and slowly dripping 50ml of NaOH solution with the concentration of 2mol/L under the stirring state to obtain a mixed solution;
(2) stirring the mixed solution in a thermostatic water bath at 60 ℃ for 3h to slowly mineralize chitosan on the surface of the XDK to form chitosan gel, adjusting the chitosan gel to be neutral, aging for 20h, and drying at 80 ℃ for 50h to obtain the chitosan adsorbent XDK-CSK.
50kg of deteriorated insulating oil to be treated was poured into an oil storage tank, 2kg of the chitosan adsorbent XDK-CSK prepared in this comparative example was cut and placed in an adsorption tank, the deteriorated insulating oil was adsorbed at a flow rate of 100L/min at 60 ℃ for 6 hours in a sealed cycle, and then the insulating oil in the filtration system was discharged.
Comparative example 2
Example 1 of the specific embodiment of patent application CN202010801826.3, as comparative example 2 of the present invention, is a process for the preparation of an adsorbent comprising the following steps:
s1, dissolving 0.625kg of chitosan powder with the weight-average molecular weight of 120 ten thousand and the deacetylation degree of more than 85% in 25L of glacial acetic acid aqueous solution with the volume fraction of 1% to obtain a chitosan solution with the concentration of 25 g/L: then 0.3125kg of XDK powder which is soaked and modified by sulfuric acid with the volume fraction of 20% is dispersed in pure water with the mass of 4 times that of the XDK powder to obtain XDK powder suspension;
s2, adding 0.1875kg of glycerol into the chitosan solution, and uniformly stirring in a stirrer to obtain a first solution;
s3, slowly adding a silicon-aluminum gel XDK adsorbent powder suspension into the first solution under the stirring state of 100r/min, and uniformly stirring to obtain a second mixed solution;
and S4, pouring the second mixed solution into a mold, freezing for 5-6h at-2-5 ℃, and finally, freezing and drying for about 48h at-70-80 ℃ to obtain the chitosan/silicon-aluminum gel powder composite material.
50kg of degraded transformer oil to be treated is poured into an oil storage tank, 1.5kg of the chitosan/silicon-aluminum gel composite material prepared in the comparative example is cut and then is filled into an adsorption tank, the flow rate of the degraded transformer oil is controlled at 100L/min, and the transformer oil in a decoloring system is discharged after sealed circulating adsorption is carried out for 6 hours at the temperature of 60 ℃.
The performance of the deteriorated insulating oil to be treated, the deteriorated insulating oils after the adsorption regeneration treatment of examples 1 to 4 and comparative examples 1 to 2 were respectively tested, and the test results are shown in table 1 below.
TABLE 1
Referring to table 1, it can be seen from the analysis of the test data of examples 1 to 4 and comparative examples 1 to 2 that the chitosan adsorbent prepared in example 1 was the worst in the 4 groups of examples in the adsorption regeneration treatment effect on the deteriorated insulating oil. However, as can be seen from the comparison of the test data of example 1 and comparative examples 1 and 2, the chitosan adsorbent prepared in example 1 has significantly better adsorption regeneration treatment effect on the deteriorated insulating oil than comparative examples 1 and 2, in terms of decolorization, deacidification, dielectric loss, volume resistivity, pressure resistance and the like. In addition, the production process of example 1 is simple, the process is easy to control, the production cost is low, and mass production can be performed, while the production process of comparative example 2 is complex, the process is not easy to control, the production cost is high, and mass production cannot be performed. Therefore, it can be determined that the technical effect of the technical scheme of the invention is obviously better than that of the comparative examples 1 and 2, and the technical effect of the preferred scheme of the invention is better.
The chitosan adsorbent prepared by the technical scheme of the invention has the advantages of remarkably improving the adsorption regeneration treatment effect of the deteriorated insulating oil, along with simple production process, easy control of the process and low production cost, and can realize large-scale production, thereby effectively solving the technical problems in the prior art.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. A large-scale production method of a chitosan adsorbent for regenerating deteriorated insulating oil is characterized by comprising the following steps:
(1) adding silicon-aluminum gel into chitosan gel liquid, stirring for 0.5h, and slowly dripping NaOH solution with the concentration of 2mol/L under the stirring state to obtain mixed liquid;
wherein the mass volume ratio (g/ml) of the silicon-aluminum gel to the chitosan gel liquid is 9:100, and the volume ratio of the NaOH solution to the chitosan gel liquid is 1-10: 100;
(2) stirring the mixed solution in a constant temperature water bath at 70 ℃ for 2h to slowly mineralize chitosan on the surface of the XDK to form chitosan gel, adjusting the chitosan gel to be neutral, aging for 24h, and drying to obtain the chitosan adsorbent XDK-CSK.
2. The large-scale production method according to claim 1, wherein in the step (2), the drying time is 24-48h, and the temperature is 85-95 ℃.
3. The mass production method according to claim 1, wherein in the step (2), the chitosan adsorbent XDK-CSK obtained after drying is packaged in a nylon cloth packaging bag with the length of 10cm and the width of 5 cm.
4. The mass production method as claimed in claim 3, wherein the chitosan adsorbent XDK-CSK is packaged in a specification of 100-500 g/bag.
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| CN202111490461.8A CN114100587A (en) | 2021-12-08 | 2021-12-08 | Large-scale production method of chitosan adsorbent for regeneration of deteriorated insulating oil |
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| CN202111490461.8A CN114100587A (en) | 2021-12-08 | 2021-12-08 | Large-scale production method of chitosan adsorbent for regeneration of deteriorated insulating oil |
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| CN103041787A (en) * | 2013-01-08 | 2013-04-17 | 山东大学 | Preparation method of crosslinked chitosan-manganese dioxide composite adsorbing material |
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- 2021-12-08 CN CN202111490461.8A patent/CN114100587A/en active Pending
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