CN110396733B - Solvent recovery method - Google Patents
Solvent recovery method Download PDFInfo
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- CN110396733B CN110396733B CN201810373753.5A CN201810373753A CN110396733B CN 110396733 B CN110396733 B CN 110396733B CN 201810373753 A CN201810373753 A CN 201810373753A CN 110396733 B CN110396733 B CN 110396733B
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- Prior art keywords
- waste
- solvent
- particles
- air blowing
- mixing
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- 239000002904 solvent Substances 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000011084 recovery Methods 0.000 title claims abstract description 17
- 239000002699 waste material Substances 0.000 claims abstract description 70
- 239000002245 particle Substances 0.000 claims abstract description 33
- 238000007664 blowing Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000009835 boiling Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 229920002678 cellulose Polymers 0.000 claims description 11
- 239000001913 cellulose Substances 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 229920000875 Dissolving pulp Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000005086 pumping Methods 0.000 abstract description 3
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 description 5
- 229920003043 Cellulose fiber Polymers 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920000715 Mucilage Polymers 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Images
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F13/00—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention provides a solvent recovery method, which is mainly used for recovering a solvent in waste materials and comprises the steps of crushing, mixing, dissolving out the solvent, dehydrating and filtering the waste materials. Crushing the waste material into particles with the average particle size of less than 1.5 mm; mixing, namely mixing the crushed waste with deionized water, and putting the mixture into a container, wherein the concentration of the waste mixed liquid is controlled to be 10-25%; dissolving out the solvent, namely heating the mixed solution of the waste materials, controlling the temperature to be 55-75 ℃, and simultaneously boiling and stirring the mixed solution for 25-40 minutes by adopting air blowing, so that the solvent in the waste materials can be fully dissolved out; and (4) dewatering and filtering, namely pumping the waste mixed liquid into a dewatering machine for dewatering, collecting filtrate, and separating waste particles. The method of the invention is adopted to recover the solvent in the waste material, the recovery rate of the solvent reaches 99.99 percent, and the production cost is obviously reduced.
Description
Technical Field
The invention relates to a solvent recovery method, and belongs to the technical field of cellulose fibers.
Background
The solvent method cellulose fiber is prepared by mixing cellulose and a solvent, particularly an NMMO solvent, dissolving in a dissolving device to prepare a cellulose glue solution, and then spinning by dry-jet wet spinning. In the solvent method cellulose fiber production, especially in the process of starting a process system, cellulose mucilage needs to be discharged, and the discharged cellulose mucilage is solidified in the environment of air and water to form waste. The waste contains a large amount of solvent, and the solvent in the waste needs to be recovered and recycled after purification treatment, so that the production raw materials are saved, the pollution is reduced, and the production cost is reduced.
The existing solvent recovery methods simply soak the waste material with deionized water, the solvent entering the water by diffusion. By adopting the method, the solvent in the waste material can not be dissolved out completely, the recovery rate is only about 60-70%, and a large amount of solvent is lost.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a solvent recovery method, which aims to realize the purposes of efficiently recovering the solvent in the waste, reducing the production cost and reducing the pollution.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a solvent recovery method is characterized in that the solvent is a solvent capable of dissolving cellulose, preferably an NMMO solvent, the waste material is a glue solution prepared by a cellulose/solvent system, and the waste material is solidified and preferably cellulose/NMMO system waste material. The invention relates to a method for preparing a high-concentration solvent-containing waste material, which comprises the steps of crushing the waste material containing the high-concentration solvent into particles with a certain particle size, mixing the particles with deionized water, and putting the mixture into a container with the functions of air-blowing boiling stirring and heating. The method adopts a container with air blowing and heating functions to heat, air-blow, boil and stir the waste mixed liquid, and controls the concentration, the temperature and the time to fully dissolve out and recycle the solvent in the waste.
The method comprises the following specific implementation steps:
(1) The waste material, mainly glue solution prepared by a cellulose/solvent system, is solidified into waste material, preferably cellulose/NMMO system waste material, and is crushed into particles with the average particle size of less than 1.5 mm.
(2) The crushed waste particles are mixed with deionized water and then put into a container. A steam heating pipe is arranged in the container, a plurality of steam holes with the aperture of 1-1.5mm are uniformly distributed on the steam heating pipe, and steam can be sprayed out from the steam holes; the container is provided with a compressed air blowing pipe, a plurality of air blowing holes with the aperture of 1-1.5mm are uniformly distributed on the compressed air blowing pipe, and the compressed air can be sprayed out from the air blowing holes.
(3) And controlling the concentration of the waste mixed liquor in the container to be 10-25%. Heating the waste mixed liquor, and controlling the temperature at 55-75 ℃. Meanwhile, the mixed solution is boiled and stirred for 25-40 minutes by air blowing, and the solvent in the waste can be fully dissolved out.
(4) And pumping the waste mixed solution after the solvent is dissolved into a dehydrator through a centrifugal pump for dehydration and filtration, collecting filtrate, and separating waste particles.
(5) And (4) washing the waste particles, washing the waste particles of the dehydrator for 10-15 minutes by using deionized water, and collecting washing liquid containing the solvent.
(6) And finally, dehydrating and filtering the waste particles, and respectively collecting filtrate and the waste particles.
By adopting the method, the solvent content of the waste particles is less than 0.01 percent, and the recovery rate of the solvent in the waste reaches more than 99.99 percent.
Due to the adoption of the technical scheme, the invention achieves the technical effects that:
the invention recovers the solvent from the waste material, the recovery rate of the solvent reaches 99.99 percent, and the production cost is obviously reduced.
Drawings
FIG. 1 is a schematic diagram of solvent recovery according to the present invention.
Detailed Description
The present invention will be described in detail with reference to examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be apparent to those skilled in the art that several modifications and improvements can be made without departing from the inventive concept. All falling within the scope of the present invention.
Example 1A solvent recovery method
The method comprises the following steps:
(1) Comminution of waste materials
The waste material, which is mainly a glue solution prepared from a cellulose/solvent system, is coagulated, preferably a cellulose/NMMO system waste material, and is crushed into particles with an average particle size of 1.3 mm.
(2) Mixing of
Mixing the crushed waste particles with deionized water, putting the mixture into a container with functions of air-blowing boiling stirring and heating, and controlling the concentration of waste mixed liquid to be 22%.
The container is provided with a compressed air blowing pipe and a steam heating pipe, and the compressed air blowing pipe and the steam heating pipe are respectively and uniformly distributed with air blowing holes and steam holes with the aperture of 1 mm.
(3) Solvent dissolution
And introducing steam into the steam heating pipe, spraying the steam from the steam holes, heating the waste particle mixed solution, controlling the temperature at 63 ℃, introducing compressed air into the compressed air blowpipe, spraying the compressed air from the air blowing holes, carrying out air blowing boiling stirring on the waste mixed solution for 25 minutes, and fully dissolving out the solvent in the waste particles under the control of the concentration, the temperature and the time.
(4) Dewatering and filtering
And pumping the waste mixed liquid after the solvent is dissolved out into a dehydrator through a centrifugal pump, dehydrating and filtering, and collecting filtrate.
(5) Flushing waste particles
After dehydration, the waste particles in the dehydrator were rinsed with deionized water for 10 minutes, and the washing solution was collected.
(6) Re-dewatering and filtering
And finally, dehydrating and filtering the waste particles again, and respectively collecting filtrate and the waste particles.
By adopting the method, the solvent content of the waste particles is 0.006 percent, and the recovery rate of the solvent in the waste reaches 99.994 percent.
Unless otherwise stated, the percentages used in the present invention are percentages by weight, and the proportions described in the present invention are proportions by mass.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (2)
1. A solvent recovery method, characterized by: recovering the solvent in the waste;
the solvent is a solvent capable of dissolving cellulose; the waste material is a glue solution prepared by a cellulose/solvent system and is solidified into a waste material;
the solvent recovery method comprises the steps of crushing and mixing the waste, dissolving out the solvent, dehydrating and filtering, and washing waste particles;
crushing the waste into particles with the average particle size of less than 1.5 mm;
mixing, namely mixing the crushed waste with deionized water, and putting the mixture into a container, wherein the concentration of the waste mixed liquid in the container is controlled to be 10-25%;
the container is provided with a compressed air blowing pipe, a plurality of air blowing holes with the aperture of 1-1.5mm are uniformly distributed on the compressed air blowing pipe, and compressed air can be sprayed out from the air blowing holes;
the container is provided with a steam heating pipe, a plurality of steam holes with the aperture of 1-1.5mm are uniformly distributed on the steam heating pipe, and steam can be sprayed out from the steam holes;
and (3) dissolving out the solvent, namely heating the mixed liquid of the waste materials, controlling the temperature to be 55-75 ℃, and simultaneously boiling and stirring the mixed liquid for 25-40 minutes by adopting air blowing, so that the solvent in the waste materials can be fully dissolved out.
2. A solvent recovery process according to claim 1, wherein: the step of dehydration filtration, which is to pump the waste mixed solution after the solvent is dissolved out into a dehydrator through a centrifugal pump for dehydration filtration, collect filtrate and separate waste particles; washing the waste particles, washing the waste particles of the dehydrator for 10-15 minutes by using deionized water, and collecting washing liquid containing a solvent; and finally, dehydrating and filtering the waste particles, and respectively collecting filtrate and the waste particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810373753.5A CN110396733B (en) | 2018-04-24 | 2018-04-24 | Solvent recovery method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810373753.5A CN110396733B (en) | 2018-04-24 | 2018-04-24 | Solvent recovery method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110396733A CN110396733A (en) | 2019-11-01 |
| CN110396733B true CN110396733B (en) | 2022-11-25 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810373753.5A Active CN110396733B (en) | 2018-04-24 | 2018-04-24 | Solvent recovery method |
Country Status (1)
| Country | Link |
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| CN (1) | CN110396733B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224564A (en) * | 2012-01-30 | 2013-07-31 | 山东光大科技发展有限公司 | Production technology for high-substituted polyanionic cellulose by slurry method with low solvent consumption |
| CN104711706A (en) * | 2015-03-17 | 2015-06-17 | 中国纺织科学研究院 | Lyocell fiber spinning solution waste recycling device and recycling method thereof |
| CN106283276A (en) * | 2016-08-30 | 2017-01-04 | 中国纺织科学研究院 | The recovery method of N methylmorpholineoxide during solvent method production cellulose |
| CN107098982A (en) * | 2017-05-03 | 2017-08-29 | 浙江中维药业股份有限公司 | The production method of hydroxypropyl methylcellulose |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3124501A1 (en) * | 2009-03-09 | 2017-02-01 | TreeToTextile AB | Shaped cellulose manufacturing process |
-
2018
- 2018-04-24 CN CN201810373753.5A patent/CN110396733B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224564A (en) * | 2012-01-30 | 2013-07-31 | 山东光大科技发展有限公司 | Production technology for high-substituted polyanionic cellulose by slurry method with low solvent consumption |
| CN104711706A (en) * | 2015-03-17 | 2015-06-17 | 中国纺织科学研究院 | Lyocell fiber spinning solution waste recycling device and recycling method thereof |
| CN106283276A (en) * | 2016-08-30 | 2017-01-04 | 中国纺织科学研究院 | The recovery method of N methylmorpholineoxide during solvent method production cellulose |
| CN107098982A (en) * | 2017-05-03 | 2017-08-29 | 浙江中维药业股份有限公司 | The production method of hydroxypropyl methylcellulose |
Non-Patent Citations (1)
| Title |
|---|
| 天丝织物染整的清洁生产;张如美;《环境导报》;20030130(第06期);第32-33页 * |
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| CN110396733A (en) | 2019-11-01 |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20210521 Address after: Room 1115, Zhongfu building, 99 Jianguo Road, Chaoyang District, Beijing 100020 Applicant after: HI-TECH FIBER Group Corp. Applicant after: BAODING SWAN FIBER CO.,LTD. Address before: Room 1115, Zhongfu building, 99 Jianguo Road, Chaoyang District, Beijing 100020 Applicant before: HI-TECH FIBER Group Corp. Applicant before: BAODING SWAN FIBER CO.,LTD. Applicant before: CHTC BIO-BASED MATERIAL ENGINEERING & TECHNOLOGY(NINGBO) Co.,Ltd. |
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Effective date of registration: 20231207 Address after: 072250 North of Gaosheng Pu Village, Pushang Town, Shunping County, Baoding City, Hebei Province (east side of Zhangshi Expressway lead) Patentee after: BAODING SWAN FIBER CO.,LTD. Address before: Room 1115, Zhongfu building, 99 Jianguo Road, Chaoyang District, Beijing 100020 Patentee before: HI-TECH FIBER Group Corp. Patentee before: BAODING SWAN FIBER CO.,LTD. |