CN102732280B - High-softening-point coal-tar pitch production method - Google Patents
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- CN102732280B CN102732280B CN201210234655.6A CN201210234655A CN102732280B CN 102732280 B CN102732280 B CN 102732280B CN 201210234655 A CN201210234655 A CN 201210234655A CN 102732280 B CN102732280 B CN 102732280B
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Abstract
The invention relates to a high-softening-point coal-tar pitch production method, which is mainly and technically characterized in that the method comprises the following steps of: (1) adding low-QI (Quality Index) purified coal-tar pitch into a stirring tank, continuously feeding air into the stirring tank, carrying out stirring in the process of feeding air, and carrying out air oxidation under the condition of 200-300 DEG C, wherein the oxidation time is 4-12 h; and (2) after the oxidation is completed, adding the pitch into a film evaporator, carrying out thin-film distillation on the pitch at a temperature of 300-350 DEG C and under a vacuum negative pressure of 0.05-0.099 Mpa, removing light components in the pitch, and carrying out distillation treatment on the obtained product for one to four hours so as to obtain high-softening-point coal-tar pitch. The method disclosed by the invention is reasonable in design; and the softening point of high-softening-point coal-tar pitch produced by taking the low-QI purified coal-tar pitch as raw materials reaches 270-290 DEG C, and the high-softening-point coal-tar pitch is low in impurity content, high in purity, simple in production process, energy-saving and environmental-friendly, and can be widely applied to the production of cathode materials jackets for lithium ion batteries and carbon fibers.
Description
Technical field
The invention belongs to technical field of coal chemical industry, relate in particular to a kind of production method of high softening-point coal-tar pitch.
Background technology
Because high softening point bitumen has superior high-temperature resistance, thereby obtained application more widely.Conventionally preparation method's more complicated of high softening point bitumen, have relatively high expectations, subsequent disposal complexity, the simultaneously too high application performance that more can affect pitch of QI value.When high softening point bitumen is used for lithium ion battery negative coating material, coated rear graphite granule is easy to the destruction that comes off that is easy to cause coating layer in bonding pulverization process afterwards, affects the overall performance of negative material; While being used for the spinning raw material of carbon fiber, the too high performance that can have a strong impact on carbon fiber of QI.
The production of high softening point bitumen is mainly to realize by oxidizing process and solvent de-asphalting process.Solvent de-asphalting process exists that energy consumption is large, heating coking problem is serious, viscosity causes greatly the problems such as discharging difficulty, and traditional oxidized bitumen technique exist oxidation efficiency low, be oxidized the problems such as inhomogeneous.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of production method of reasonable in design, oxidation efficiency is high, oxidation is even and product QI value is low high softening-point coal-tar pitch is provided.
The present invention solves its technical problem and takes following technical scheme to realize:
A production method for high softening-point coal-tar pitch, comprises the following steps:
(1) low QI is purified to coal-tar pitch and join in stirring tank, and continuously pass into air, in venting process, stir, under 200～300 ℃ of conditions, carry out atmospheric oxidation, oxidization time is 4～12h;
(2) pitch after oxidation is joined in thin-film evaporator, under 300～350 ℃, negative pressure of vacuum 0.05～0.099MPa condition, carry out thin film distillation, remove light constituent, then distill processing, obtain high softening point bitumen after distilling 1～4h.
And the low QI that (1) described step used purifies QI≤0.3% of coal-tar pitch, softening temperature is 80～90 ℃, coking value >=46%, TI >=12%.
And the softening temperature of described high softening point bitumen is 270～290 ℃, coking value >=70%, QI≤25%.
And, the preparation method that described low QI purifies coal-tar pitch is: mid-temperature pitch is circulated and joined in molecular still by recycle pump, cycle rate is 400～600ml/min, in negative pressure of vacuum, be that 0.01～0.1MPa, distillation initial temperature are that 130～180 ℃, distillation and the condensation temperature difference are to distill under 40～80 ℃ of conditions, in still-process, constantly heat up, temperature rise rate is 2～6 ℃/min, when distillation temperature rises to 310～380 ℃, obviously cut output of nothing in distiller, distillation stops, and removes to obtain low QI after residue and purify coal-tar pitch.
Advantage of the present invention and positively effect are:
The present invention is reasonable in design, it adopts low QI purification coal-tar pitch to carry out oxide treatment and adopt thin-film evaporator to carry out thin film distillation processing as raw material, the softening temperature of the high softening point bitumen that production obtains has reached 270～290 ℃, coking value >=70%, QI≤25%, and high softening-point coal-tar pitch foreign matter content is few, purity is high, production technique is simple, energy-conserving and environment-protective, can be widely used in the production of the coated and carbon fiber of lithium ion battery negative material.
Embodiment
Below in conjunction with example, the present invention is described further.
A production method for high softening-point coal-tar pitch, comprises the following steps:
1, low QI is purified to coal-tar pitch and join in stirring tank, and continuously pass into air, in venting process, stir, under 200～300 ℃ of conditions, carry out atmospheric oxidation, oxidization time is 4～12h.
In this step, use low QI to purify coal-tar pitch as raw material, this low QI purifies QI≤0.3% of coal-tar pitch, and softening temperature is 80～90 ℃, coking value >=46%, TI >=12%.This low QI purification coal-tar pitch can be adopted with the following method and prepare:
Mid-temperature pitch is circulated and joined in molecular still by recycle pump, cycle rate is 400～600ml/min, in negative pressure of vacuum, be that 0.01～0.1MPa, distillation initial temperature are that 130～180 ℃, distillation and the condensation temperature difference are to distill under 40～80 ℃ of conditions, in still-process, constantly heat up, temperature rise rate is 2～6 ℃/min, when distillation temperature rises to 310～380 ℃, and obviously cut output of nothing in distiller, distillation stops, and removes to obtain low QI after residue and purify coal-tar pitch.
2, pitch after oxidation is joined in thin-film evaporator, under 300～350 ℃, negative pressure of vacuum 0.05～0.099MPa condition, carry out thin film distillation, remove light constituent, then distill processing, after distillation 1～4h, obtain high softening point bitumen, the softening temperature of gained high softening-point coal-tar pitch is 270～290 ℃, coking value >=70%, QI≤25%.
Embodiment 1:
Low QI is purified to coal-tar pitch and join in stirring tank, and continuously pass into air, in venting process, stir, under 250 ℃ of conditions, carry out atmospheric oxidation, oxidization time 6h; Then pitch after oxidation is joined in thin-film evaporator, under 320 ℃, negative pressure of vacuum 0.06MPa condition, carry out thin film distillation, remove light constituent, after distillation time 2h, complete distillation processing and obtain high softening point bitumen, the softening temperature of gained high softening-point coal-tar pitch is 270～290 ℃, coking value >=70%, QI≤25%, reaches expectation product standard.
Embodiment 2:
Low QI is purified to coal-tar pitch and join in stirring tank, and continuously pass into air, in venting process, stir, under 260 ℃ of conditions, carry out atmospheric oxidation, oxidization time 6.5h; Then pitch after oxidation is joined in thin-film evaporator, under 330 ℃, negative pressure of vacuum 0.07MPa condition, carry out thin film distillation, remove light constituent, after distillation time 2.5h, complete distillation processing and obtain high softening point bitumen, the softening temperature of gained high softening-point coal-tar pitch is 270～290 ℃, coking value >=70%, QI≤25%, reaches expectation product standard.
Embodiment 3:
Low QI is purified to coal-tar pitch and join in stirring tank, and continuously pass into air, in venting process, stir, under 270 ℃ of conditions, carry out atmospheric oxidation, oxidization time 7h; Then pitch after oxidation is joined in thin-film evaporator, under 340 ℃, negative pressure of vacuum 0.08MPa condition, carry out thin film distillation, remove light constituent, distillation time 3h, complete distillation processing and obtain high softening point bitumen, the softening temperature of gained high softening-point coal-tar pitch is 270～290 ℃, coking value >=70%, QI≤25%, reaches expectation product standard.
It is emphasized that; embodiment of the present invention is illustrative; rather than determinate; therefore the present invention is not limited to the embodiment described in embodiment; every other embodiments that drawn by those skilled in the art's technical scheme according to the present invention, belong to the scope of protection of the invention equally.
Claims (4)
1. a production method for high softening-point coal-tar pitch, is characterized in that: comprise the following steps:
(1) low QI is purified to coal-tar pitch and join in stirring tank, and continuously pass into air, in venting process, stir, under 200～300 ℃ of conditions, carry out atmospheric oxidation, oxidization time is 4～12h;
(2) pitch after oxidation is joined in thin-film evaporator, under 300～350 ℃, negative pressure of vacuum 0.05～0.099MPa condition, carry out thin film distillation, remove light constituent, then distill processing, obtain high softening point bitumen after distilling 1～4h;
Described low QI purifies QI≤0.3% of coal-tar pitch; The softening temperature of described high softening point bitumen is 270～290 ℃.
2. the production method of a kind of high softening-point coal-tar pitch according to claim 1, is characterized in that: the softening temperature that described low QI purifies coal-tar pitch is 80～90 ℃, coking value >=46%, TI >=12%.
3. the production method of a kind of high softening-point coal-tar pitch according to claim 1, is characterized in that: coking value >=70% of described high softening point bitumen, QI≤25%.
4. according to the production method of a kind of high softening-point coal-tar pitch described in claims 1 to 3 any one, it is characterized in that: the preparation method that described low QI purifies coal-tar pitch is: mid-temperature pitch is circulated and joined in molecular still by recycle pump, cycle rate is 400～600ml/min, in negative pressure of vacuum, be 0.01～0.1MPa, distillation initial temperature is 130～180 ℃, distillation is to distill under 40～80 ℃ of conditions with the condensation temperature difference, in still-process, constantly heat up, temperature rise rate is 2～6 ℃/min, when distillation temperature rises to 310～380 ℃, obviously cut output of nothing in distiller, distillation stops, after removing residue, obtain low QI purification coal-tar pitch.
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| CN201210234655.6A CN102732280B (en) | 2012-07-09 | 2012-07-09 | High-softening-point coal-tar pitch production method |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103804926B (en) * | 2012-11-07 | 2016-03-30 | 中国石油化工股份有限公司 | A kind of Asphalt composition particle and preparation method thereof |
| CN103897714B (en) * | 2014-01-09 | 2016-02-24 | 湛江市聚鑫新能源有限公司 | A kind of method of the high softening point bitumen for the preparation of coated lithium ion battery natural graphite negative electrode material |
| CN106893604A (en) * | 2015-12-18 | 2017-06-27 | 上海宝钢化工有限公司 | A kind of low energy consumption and the efficiently asphalt production process of raising asphalt softening point |
| CN106281393A (en) * | 2016-08-31 | 2017-01-04 | 山东晨阳新型碳材料股份有限公司 | The Production method of coal pitch of the low quinoline insolubles of high coking value |
| CN112592734A (en) * | 2020-11-24 | 2021-04-02 | 新疆中碳新材料科技有限责任公司 | Continuous production method of lithium ion battery cathode coating material |
| CN114752397B (en) * | 2021-11-12 | 2023-07-14 | 中国神华煤制油化工有限公司 | Coated asphalt and preparation method and device thereof |
| CN114497462A (en) * | 2022-01-24 | 2022-05-13 | 中钢集团鞍山热能研究院有限公司 | Preparation method and device of coating asphalt for high-performance lithium ion battery negative electrode material |
| CN115072699B (en) * | 2022-06-29 | 2024-01-12 | 鞍钢化学科技有限公司 | Low-cost coal tar pitch-based foam carbon and preparation method of precursor thereof |
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| JPS6065090A (en) * | 1983-09-20 | 1985-04-13 | Agency Of Ind Science & Technol | Preparation of pitch for carbon fiber spinning |
| JPS62133121A (en) * | 1985-12-04 | 1987-06-16 | Nippon Oil Co Ltd | Production of pitch carbon fiber |
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| US3718493A (en) * | 1968-06-04 | 1973-02-27 | Great Lakes Carbon Corp | Process for the production of carbon filaments from coal tar pitch |
| CN101323788A (en) * | 2008-07-31 | 2008-12-17 | 上海奥韦通工程技术有限公司 | Processing process for preparing various asphalt and fuel oil with coal tar |
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Effective date of registration: 20190515 Address after: 300457 Songshan Road, Hangu Modern Industrial Zone, Tianjin Development Zone, Binhai New Area, Tianjin Patentee after: Tianjin Hexingtan Chemical Co., Ltd. Address before: B.C.D. Block, 11 storeys, Tianjin International Development Building, No. 2 Dongting Road, Tanggu Development Zone, Tianjin, 300347 Patentee before: Yu Bingwu |
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Effective date of registration: 20190606 Address after: 300457 days Tianjin Binhai New Area Tianjin Economic and Technological Development Zone Nangang Industrial Zone Planned Road East and South of Nandi Road Patentee after: Tianjin Yufeng carbon fiber products Co., Ltd. Address before: 300457 Songshan Road, Hangu Modern Industrial Zone, Tianjin Development Zone, Binhai New Area, Tianjin Patentee before: Tianjin Hexingtan Chemical Co., Ltd. |
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Effective date of registration: 20190628 Address after: 017020 Equipment Manufacturing Base F-06-01, Dongsheng District, Ordos City, Inner Mongolia Autonomous Region Patentee after: Inner Mongolia Longtong Carbon Fiber Technology Co., Ltd. Address before: 300457 days Tianjin Binhai New Area Tianjin Economic and Technological Development Zone Nangang Industrial Zone Planned Road East and South of Nandi Road Patentee before: Tianjin Yufeng carbon fiber products Co., Ltd. |
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