CN114031217A - Method for rapidly treating waste oil agent for carbon fiber spinning - Google Patents
Method for rapidly treating waste oil agent for carbon fiber spinning Download PDFInfo
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- CN114031217A CN114031217A CN202111404681.4A CN202111404681A CN114031217A CN 114031217 A CN114031217 A CN 114031217A CN 202111404681 A CN202111404681 A CN 202111404681A CN 114031217 A CN114031217 A CN 114031217A
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- waste oil
- oil agent
- carbon fiber
- solution obtained
- fiber spinning
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a method for quickly treating waste oil agent for carbon fiber spinning, which comprises the following steps: heating the spinning waste oil agent in water bath at 50-75 ℃; FeSO4·7H2Dissolving O in the solution obtained in the step 1, and fully stirring; taking H with the mass fraction of 27%2O2Dropwise adding the solution obtained in the step (2) at the rate of 1 drop/second, after the continuous stirring reaction is finished, dropwise adding alkali liquor into the solution obtained in the step (3), adjusting the pH to 7-8, standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate. The method treats the waste oil agent for spinning by a Fenton oxidation method which is simple to operate, and solves the key problems of high cost and low treatment efficiency of the waste oil agent in the carbon fiber production process.
Description
Technical Field
The invention belongs to the technical field of waste oil agent treatment, and particularly relates to a method for rapidly treating carbon fiber spinning waste oil agent.
Background
The oiling agent is an important auxiliary agent in the production process of the high-performance polyacrylonitrile carbon fiber, and the oiling agent can form a film on the surfaces of monofilaments uniformly, so that the monofilaments can be prevented from being adhered and doubled, and the fiber surfaces can be prevented from being rubbed and abraded in the production process, thereby effectively avoiding the defects on the fiber surfaces, and being an effective technical measure for improving the performances of the precursor and the carbon fiber. However, with continuous production and key process characteristics of carbon fiber materials, the production amount of waste oil agents is gradually increased, and certain pressure is brought to the ecological environment. The industrial process is mainly carried out by a professional waste disposal facility by adopting a high-temperature incineration method, and the method is expensive in treatment cost and is not environment-friendly.
Disclosure of Invention
The invention aims to provide a method for quickly and efficiently treating waste oil agent for spinning in the carbon fiber production process aiming at the defects and the defects of the prior art, and solves the key problems of high treatment cost and low efficiency of the waste oil agent in the carbon fiber industry.
In order to achieve the above purpose, the present invention can be realized by the following scheme:
a method for rapidly treating carbon fiber spinning waste oil agent comprises the following steps:
(1) weighing spinning waste oil into a container, stirring at low speed, and heating in water bath at 50-75 ℃;
(2) weighing FeSO4·7H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) weighing 27% of H by mass fraction2O2Dropwise adding the mixture into the solution obtained in the step (2) at the speed of 1 drop/second, and continuously stirring;
(4) after the reaction is finished, dropwise adding alkali liquor into the solution obtained in the step (3), and adjusting the pH to 7-8;
(5) and (4) standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate.
Further, FeSO4·7H2The amount of O is 0.001-0.01 a, H2O2The dosage is 0.05-0.2 a, wherein a is equal to the mass of the waste oil agent.
Compared with the prior art, the invention has the following advantages:
1. the cost is low, and the treatment efficiency is high;
2. the treatment process is quick, and the operation is simple;
3. is environment-friendly.
Detailed Description
The embodiment of the invention is used for quickly and efficiently treating the waste oil agent generated in the carbon fiber spinning process by a simple Fenton oxidation method, and the high-efficiency treatment of the waste oil agent can be realized by controlling the reaction temperature, the hydrogen peroxide dosage, the ferric salt dosage and other process conditions. The following provides a detailed description of specific embodiments of the present invention.
The method has strong applicability and high application value, and can be popularized and used in the post-treatment of the waste oil agent in the silicon oil agent industry.
Therefore, the method for treating the spinning waste oil agent by the Fenton oxidation method is an efficient and rapid treatment method, effectively reduces the Chemical Oxygen Demand (COD), reduces the treatment cost of the waste oil agent and protects the environment. The method can be applied to different fields relating to silicon oil agents.
Example 1
(1) Weighing 250g of spinning waste oil agent into a four-neck flask, stirring at a low speed, and heating in a water bath at 65 ℃;
(2) 0.75g of FeSO was weighed4·7H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) 37.5g of 27% H are weighed out2O2Dropwise adding the solution obtained in the step (2) at the speed of 1 drop/second, and continuously stirring;
(4) after the reaction is finished, dropwise adding 30g/mL NaOH into the solution obtained in the step (3), and adjusting the pH value to 7;
(5) standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate;
through detection, when the method is used for treating the waste oil agent, the COD removal rate reaches 89.5%, and the solution is clear and transparent after standing and settling for 2.1 hours.
Example 2
(1) Weighing 250g of spinning waste oil agent into a four-neck flask, stirring at low speed, and heating in water bath at 60 ℃;
(2) 0.75g of FeCl was weighed3·6H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) 37.5g of 27% H are weighed out2O2Dropwise adding the mixture into the solution obtained in the step (2) at the speed of 1 drop/second, and continuously stirring;
(4) after the reaction is finished, dropwise adding 30g/mL NaOH into the solution obtained in the step (3), and adjusting the pH value to 7;
(5) standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate;
through detection, the COD removal rate of the waste oil agent treated by the method reaches 72.1%, and the solution is yellow and transparent after standing and settling for 4 hours.
Example 3
(1) Weighing 250g of spinning waste oil agent into a four-neck flask, stirring at low speed, and heating in water bath at 55 ℃;
(2) 0.75g of FeSO was weighed4·7H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) 18.75g of 27% H are weighed out2O2Dropwise adding the mixture into the solution obtained in the step (2) at the speed of 1 drop/second, and continuously stirring;
(4) after the reaction is finished, dropwise adding 30g/mL NaOH into the solution obtained in the step (3), and adjusting the pH value to 7;
(5) standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate;
through detection, when the method is used for treating the waste oil agent, the COD removal rate reaches 85.2%, and the solution is clear and transparent after standing and settling for 5.4 hours.
Example 4
(1) Weighing 250g of spinning waste oil agent into a four-neck flask, stirring at low speed, and heating in water bath at 70 ℃;
(2) 1.5g of FeSO are weighed4·7H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) 37.5g of 27% H are weighed out2O2Dropwise adding the mixture into the solution obtained in the step (2) at the speed of 1 drop/second, and continuously stirring;
(4) after the reaction is finished, dropwise adding 30g/mL NaOH into the solution obtained in the step (3), and adjusting the pH value to 7;
(5) standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate;
through detection, when the method is used for treating the waste oil agent, the COD removal rate reaches 81.6%, and the solution is yellow and transparent after standing and settling for 4.6 hours.
Example 5
(1) Weighing 250g of spinning waste oil agent into a four-neck flask, stirring at low speed, and heating in water bath at 50 ℃;
(2) 0.38g of FeSO was weighed4·7H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) 18.75g of 27% H are weighed out2O2Dropwise adding the mixture into the solution obtained in the step (2) at the speed of 1 drop/second, and continuously stirring;
(4) after the reaction is finished, dropwise adding 30g/mL NaOH into the solution obtained in the step (3), and adjusting the pH value to 7;
(5) standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate;
through detection, when the method is used for treating the waste oil agent, the COD removal rate reaches 76.8%, and the solution is yellow and opaque after standing and settling for 6 hours.
Example 6
(1) Weighing 250g of spinning waste oil agent into a four-neck flask, stirring at a low speed, and heating in a water bath at 75 ℃;
(2) 1.5g of FeSO are weighed4·7H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) 75g of 27% H are weighed out2O2Dropwise adding the mixture into the solution obtained in the step (2) at the speed of 1 drop/second, and continuously stirring;
(4) after the reaction is finished, dropwise adding 30g/mL NaOH into the solution obtained in the step (3), and adjusting the pH value to 7;
(5) standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate;
through detection, when the method is used for treating the waste oil agent, the COD removal rate reaches 90.6%, and the solution is clear and transparent after standing and settling for 1.8 hours.
Example 7
(1) Weighing 250g of spinning waste oil agent into a four-neck flask, stirring at low speed, and heating in water bath at 60 ℃;
(2) 0.75g of FeSO was weighed4·7H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) 75g of 27% H are weighed out2O2Dropwise adding the mixture into the solution obtained in the step (2) at the speed of 1 drop/second, and continuously stirring;
(4) after the reaction is finished, dropwise adding 30g/mL NaOH into the solution obtained in the step (3), and adjusting the pH value to 7;
(5) standing the solution obtained in the step (4) for 30-50min, and performing suction filtration to obtain a filtrate;
through detection, when the method is used for treating the waste oil agent, the COD removal rate reaches 78.4%, and the solution is clear and transparent after standing and settling for 3.5 hours.
The foregoing embodiments are merely illustrative of the present invention and are not limiting, and modifications, substitutions, and variations may be made thereto without departing from the spirit and scope of the invention.
Claims (8)
1. A method for rapidly treating waste oil agent for carbon fiber spinning is characterized by comprising the following steps:
(1) weighing spinning waste oil into a container, stirring at low speed, and heating at 50-75 ℃;
(2) weighing FeSO4·7H2Dissolving O in the solution obtained in the step (1), and fully stirring;
(3) weighing 27% of H by mass fraction2O2Dropwise adding the mixture into the solution obtained in the step (2), and continuously stirring;
(4) after the reaction is finished, dropwise adding alkali liquor into the solution obtained in the step (3), and adjusting the pH to 7-8;
(5) and (4) standing the solution obtained in the step (4), and performing suction filtration to obtain a filtrate.
2. The method for rapidly processing the waste oil agent for carbon fiber spinning according to claim 1, characterized in that: and (1) selecting a water bath heating mode for heating.
3. The method for rapidly processing the waste oil agent for carbon fiber spinning according to claim 1, characterized in that: in step (2), FeSO4·7H2The dosage of O is 0.001-0.01 a, wherein a is equal to the mass of the waste oil agent.
4. The method for rapidly processing the waste oil agent for carbon fiber spinning according to claim 1, characterized in that: in the step (3), the mass fraction of H is 27%2O2The dosage is 0.05-0.2 a, wherein a is equal to the mass of the waste oil agent.
5. The method for rapidly processing the waste oil agent for carbon fiber spinning according to claim 1, characterized in that: in the step (3), the dropping rate was 1 drop/sec.
6. The method for rapidly processing the waste oil agent for carbon fiber spinning according to claim 1, characterized in that: in the step (4), the alkali liquor is NaOH solution with the mass concentration of 30 g/mL.
7. The method for rapidly processing the waste oil agent for carbon fiber spinning according to claim 1, characterized in that: in the step (4), the standing time is 30-50 min.
8. The method for rapidly processing the waste oil agent for carbon fiber spinning according to claim 1, characterized in that: the container is a four-mouth flask.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202111404681.4A CN114031217A (en) | 2021-11-24 | 2021-11-24 | Method for rapidly treating waste oil agent for carbon fiber spinning |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111404681.4A CN114031217A (en) | 2021-11-24 | 2021-11-24 | Method for rapidly treating waste oil agent for carbon fiber spinning |
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| CN114031217A true CN114031217A (en) | 2022-02-11 |
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Citations (6)
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|---|---|---|---|---|
| WO2006019321A1 (en) * | 2004-08-20 | 2006-02-23 | United Environmental Limited | Improvements in and relating to waste treatment |
| CN102633322A (en) * | 2012-04-17 | 2012-08-15 | 西安建筑科技大学 | Semi-coke waste water pretreatment method based on Electro-Fenton oxidization technology |
| CN102923912A (en) * | 2012-11-07 | 2013-02-13 | 浙江大学 | Method for comprehensively treating sewage of chemical fiber oiling agents in production plants |
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2021
- 2021-11-24 CN CN202111404681.4A patent/CN114031217A/en active Pending
Patent Citations (6)
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| CN102633322A (en) * | 2012-04-17 | 2012-08-15 | 西安建筑科技大学 | Semi-coke waste water pretreatment method based on Electro-Fenton oxidization technology |
| CN102923912A (en) * | 2012-11-07 | 2013-02-13 | 浙江大学 | Method for comprehensively treating sewage of chemical fiber oiling agents in production plants |
| CN103523958A (en) * | 2013-10-13 | 2014-01-22 | 陕西盛迈石油有限公司 | High-concentration spinning oil wastewater pretreatment system |
| CN106567140A (en) * | 2016-10-27 | 2017-04-19 | 青岛大学 | Refinement production method of refined kendir fiber |
| CN108264169A (en) * | 2017-01-03 | 2018-07-10 | 黑龙江吉纳森生物工程股份有限公司 | A kind of drilling well oil-containing waste water treating device |
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| 唐建兴等: "短纤油剂废水降COD值研究", 《合成技术及应用》 * |
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Application publication date: 20220211 |
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