CN105672016A - Washing and solvent recycling method for paper pulp obtained through organic solvent method - Google Patents
Washing and solvent recycling method for paper pulp obtained through organic solvent method Download PDFInfo
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- CN105672016A CN105672016A CN201610144380.5A CN201610144380A CN105672016A CN 105672016 A CN105672016 A CN 105672016A CN 201610144380 A CN201610144380 A CN 201610144380A CN 105672016 A CN105672016 A CN 105672016A
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- organic solvent
- washing
- paper pulp
- recovering solvents
- pulping
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/02—Washing ; Displacing cooking or pulp-treating liquors contained in the pulp by fluids, e.g. wash water or other pulp-treating agents
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C11/00—Regeneration of pulp liquors or effluent waste waters
Abstract
The invention relates to a washing and solvent recycling method for paper pulp obtained through an organic solvent method.The method comprises the following steps that paper pulp obtained by pulping through the organic solvent method is washed with one or more organic solvents, then the organic solvents in the paper pulp are evaporated out through evaporation drying, dry paper pulp is obtained, and organic solvent steam is recycled through condensation.The method is suitable for washing paper pulp obtained through the organic solvent method, the organic solvents are used in the whole washing process, involvement of water is avoided, clean dry paper pulp is directly obtained through evaporation drying after washing, and the washing process of paper pulp is simplified.According to the method, due to the fact that water involvement is avoided in the whole process, energy consumption in organic solvent recycling is reduced due to the low boiling point of the organic solvents when the organic solvents are separated and recycled; in addition, azeotrope is not generated, and the trouble brought by azeotropy on organic solvent recycling is saved.
Description
Technical field
The present invention relates to the washing of a kind of solvent method boiling gained paper pulp and method for recovering solvents, solvent used to soluble substance in solid-state paper pulp fiber, waste liquid, boiling can be separated by the method one by one, and then realize the washing of paper pulp and the recovery of solvent, belong to pulp and paper technology field.
Background technology
Pulping and paper-making is conventional industries, slurrying is exactly except the most of lignin in plant material and part hemicellulose by de-, obtain the process of cellulose pulp, plant material, through chemical pulping, obtains paper pulp and waste liquid, and the paper pulp containing waste liquid obtains clean paper pulp through washing, then through bleaching, obtain pure white paper pulp, further copy paper, obtain paper or cardboard.
The method of chemical pulping can be divided into two classes, and a class utilizes the pharmaceutical chemicalss such as acid, alkali and salt to carry out pulping by cooking, and such as soda processes, sulphate process and sulphite process, this kind of method is the pulping process generally adopted existing, industrial. Another class utilizes organic solvent method to carry out pulping by cooking, such as methyl alcohol, ethanol, acetone, butanols, ethylene glycol, formic acid and acetic acid etc., organic solvent pulping temperature is generally between 120～220 DEG C, and in cooking reaction medium, the volume ratio of organic solvent is from 55～85%. Utilize with routine pharmaceutical chemicals boiling pulping process compared with, lignin in pulping waste liquor can precipitate out by simply adding the mode of water, obtain the lignin product of high purity, in addition, the organic solvent used reclaims by rectifying or other means, therefore, there is huge development potentiality.
Organic solvent pulping nineteen sixty-eight TheodorKleinert proposes (see U.S. patent documents US3585104A first, Organosolvpulpingandrecoveryprocess), but still there is no large-scale industrial application so far, its reason mainly contains two aspects, the first, organic solvent is mostly inflammable and explosive, under the High Temperature High Pressure of slurrying, the sealing of container, resistance to compression are all difficult to meet safety requirements, and initial investment is bigger, 2nd, paper pulp is difficult to adopt traditional mode of washing, if because organic solvent pulps washes with water, the lignin dissolved is deposited on paper pulp fiber again, if and wash with organic solvent, in order to meet the follow-up bleaching at aqueous phase, last section must wash with water, replace out by organic solvent, the aqueous solutions of organic solvent of big volume low-concentration can be produced like this, and the organic solvent in order to reclaim in scrub raffinate, the water added and organic solvent must be separated, this needs large-scale rectifying device, such as the separation of second alcohol and water, the alcohol concn that azeotropic point makes rectifying obtain can not higher than 95.6%,If formic acid slurrying, the boiling point of formic acid is 10.8 DEG C, and the boiling point of water is 100 DEG C, and owing to boiling point is close, distillation technology is difficult to separate both in its scrub raffinate, and rectifying energy consumption is huge. Therefore, the washing of organic solvent method paper pulp needs complicated washing plant, and washing process is huge on the recovery impact of solvent. Therefore, the washing of paper pulp is the bottleneck of restriction organic solvent pulping industrialization with the recovery of solvent in associated waste liquid.
Chinese patent document CN1417406A (application number: 01129051.X) one reclaims organic solvent method separating lignin paper pulp making technology, belongs to the processing method technical field of cellulose containing raw material organosolv pulping. It is the character utilizing xylogen to dissolve in the organic solutions such as dioxane, alcohol class, ester class, phenols, ketone class, acetyl bromide, during paper-making pulping, after paper making raw material and above-mentioned single solvent or double solvents and acid class, ammonia (amine) catalyst mix such as class, anthraquinone derivative machinery mill slurry, again through backflow dipping, boil slurry or high pressure boil slurry, mixed slurry is through pressure (mistake) filter, the fiber isolated is sized mixing copy paper, concentrating filter liquor isolates high Vinsol for deep development, organic solvent recycling. Although this patent document relates to the recovery of organic solvent, but do not relate to the washing process of paper pulp and the concrete removal process of organic solvent.
Summary of the invention
The present invention is directed to the complicated problem with difficult solvent recovery of solvent method boiling gained pulp washing process, the washing methods of a kind of simple and feasible is provided, soluble substance in solid-state paper pulp fiber, waste liquid, cooking reaction medium (solvent) can be separated by the method one by one, and then realize the washing of paper pulp and the recovery of solvent.
The technical scheme of the present invention is as follows:
The washing of organic solvent method paper pulp and a method for recovering solvents, comprise step as follows:
By organic solvent pulping gained paper pulp through one or more organic solvent washings, then evaporation drying by the organic solvent evaporation in paper pulp out, obtains dry pulp, and organic vapor is through condensation recycling.
According to the present invention, it is preferable that, described organic solvent is that methyl alcohol, ethanol, phenol, ether, butanols, ethylene glycol, acetone, formic acid, acetic acid are or/and ethyl acetate.
According to the present invention, it is preferable that, the washing times of paper pulp is more than twice;
Preferred further, it is identical with organic solvent pulping solvent for use composition that first time washs organic solvent used;
Further preferred, the organic solvent that rear once washing is used and front once washing organic solvent used are mutually miscible; Preferred, compared with the organic solvent that rear once washing organic solvent used is used with front once washing, there is lower boiling point and the latent heat of vaporization.
According to the present invention, it is preferable that, the boiling point of the temperature≤organic solvent of washing.
According to the present invention, it is preferable that, first squeeze or take out filter or centrifugal treating before organic solvent pulping gained pulp washing, to improve the mass dryness fraction of paper pulp.
According to the present invention, it is preferable that, the washing of described paper pulp, all adopts multistage counter current mode of washing, to improve detersive efficiency.
According to the present invention, it is preferable that, evaporation drying, carries out under barometric point or condition of negative pressure; Preferred further, evaporation drying temperature is lower than the boiling point of organic solvent.
According to the present invention, it is preferable that, before evaporation drying, paper pulp first squeezes or takes out filter or centrifugal treating, to improve the mass dryness fraction of paper pulp.
According to the present invention, it is preferable that, scrub raffinate after washing and organic vapor by the mode of rectifying, isolate the soluble substance in pulping process reaction medium used, washing process organic solvent used and scrub raffinate through condensed phlegma.
According to the present invention, it is preferable that, the washing of described organic solvent method paper pulp and method for recovering solvents, be applicable to washing and the solvent recuperation of the raw material organic solvent pulping gained paper pulp such as agricultural stalk, bamboo, bagasse and timber.
The washing of organic solvent method paper pulp of the present invention and method for recovering solvents comprise the rectifying separation three kinds operation of the washing of paper pulp, the evaporation drying washing rear paper pulp and process waste liquid. To use the priority of two kinds of organic solvents to wash, first, use organic solvent 1. first time washing pulp, soluble substance in paper pulp and reaction medium are transferred to scrub raffinate 1. in, then using organic solvent 2. second time washing pulp, the scrub raffinate that 2. 1. acquisition be made up of with organic solvent organic solvent is 2.; 1. and 2. 2nd, the paper pulp heat drying after twice washing, obtains dry pulp, and condensation reclaims organic solvent; 3rd, the waste liquid of whole process gained, through rectifying separation, reclaims the soluble substance in slurrying reaction medium used, pulping waste liquor and washs organic solvent used.
The useful effect of the present invention is as follows:
1, the present invention is applicable to the washing of the paper pulp that organic solvent method obtains, and washing is omnidistance uses organic solvent, avoids the participation of water, and after washing, evaporation drying directly obtains clean dry pulp, simplifies the washing process of paper pulp.
2, the present invention does not have the participation of water due to whole process, and during Separation and Recovery organic solvent, boiling point due to organic solvent is low, reduces the energy consumption reclaiming organic solvent, and can not produce azeotrope, decreases the trouble of the recovery organic solvent aspect brought because of azeotropic.
Embodiment
Below by specific embodiment, the invention will be further described, but is not limited to this.
Organic solvent purity used in embodiment is all >=99.9%.
Embodiment 1:
Taking cizu as raw material, the formic acid taking 85% carries out boiling as reaction medium, and reaction medium and raw materials quality are than being 7:1, with temperature 140 DEG C of boilings in airtight voltage-resistant reactor, reaction 120min, obtains boiling product through press filtration, obtains the cooking waste liquor that squeezes out and unwashed wet pulp.
Taking formic acid be organic solvent 1., first time pulp washing is carried out under temperature 90 DEG C of environment, with the abundant washing pulp of the form of multistage counter current, obtain scrub raffinate 1., the cooking waste liquor mixing that 1. scrub raffinate squeezes out with above-mentioned, then 50 DEG C, evaporation concentration under the negative pressure of 0.1MPpa, obtains being rich in residue and the phlegma of organism, phlegma is formic acid, can directly reaction medium as slurrying use. Paper pulp after first time washing is that 2. organic solvent carries out second time washing under 50 DEG C of conditions taking methyl alcohol, with the abundant washing pulp of the form of multistage counter current, obtain scrub raffinate 2., paper pulp after second time washing evaporates at 64 DEG C, obtain dry paper pulp and phlegma, 2. phlegma and scrub raffinate mix, rectifying separation reclaim organic solvent 2., organic solvent 1. with the cooking reaction medium of minute quantity.
Embodiment 2:
Taking wheat straw as raw material, the ethanol taking 60% carries out boiling as reaction medium, and reaction medium and raw materials quality are than being 8:1, with temperature 200 DEG C of boilings in airtight voltage-resistant reactor, reaction 120min, obtains boiling product through press filtration, obtains the waste liquid that squeezes out and unwashed wet pulp.
Take ethanol as organic solvent, under temperature 70 DEG C of environment, carry out pulp washing, with the abundant washing pulp of the form of multistage counter current, obtain scrub raffinate.Scrub raffinate and the above-mentioned waste liquid mixing squeezed out, at 78 DEG C, abundant evaporation concentration, obtains being rich in residue and the phlegma of organism, paper pulp after washing reduction vaporization at 40 DEG C is dry, obtaining dry paper pulp and phlegma, all phlegmas mix, and rectifying separation reclaims ethanol.
Embodiment 3:
Taking bagasse as raw material, the acetone taking 70% carries out boiling as reaction medium, and reaction medium and raw materials quality are than being 6:1, with 160 DEG C of boilings in airtight voltage-resistant reactor, reaction 120min, obtains boiling product through press filtration, obtains the waste liquid that squeezes out and unwashed wet pulp.
Take acetone as organic solvent, under temperature 56 DEG C of environment, carry out pulp washing, with the abundant washing pulp of the form of multistage counter current, obtain scrub raffinate. Scrub raffinate and the above-mentioned waste liquid mixing squeezed out, at 50 DEG C, abundant evaporation concentration, obtains being rich in residue and the phlegma of organism, paper pulp after washing reduction vaporization at 40 DEG C is dry, obtaining dry paper pulp and phlegma, all phlegmas mix, and rectifying separation reclaims acetone.
Embodiment 4:
Taking Yang Mu as raw material, carry out boiling taking formic acid, acetic acid, water (3:2:1) as reaction medium, reaction medium and raw materials quality are than being 6:1, temperature 120 DEG C of boilings, reaction 120min, obtains boiling product through press filtration, obtains the waste liquid that squeezes out and unwashed wet pulp.
Taking formic acid, acetic acid (3:2) as organic solvent, under temperature 100 DEG C of environment, carry out pulp washing, with the abundant washing pulp of the form of multistage counter current, obtain scrub raffinate. Scrub raffinate and the above-mentioned waste liquid mixing squeezed out, at 100 DEG C, abundant evaporation concentration, obtains being rich in residue and the phlegma of organism, paper pulp after washing reduction vaporization at 80 DEG C is dry, obtaining dry paper pulp and phlegma, all phlegmas mix, and rectifying separation reclaims acetic acid.
Embodiment 5:
Being raw material taking cizu, be that reaction medium carries out boiling taking formic acid, reaction medium and raw materials quality are than being 7:1, temperature 140 DEG C of boilings, and reaction 120min, obtains boiling product through press filtration, obtain the cooking waste liquor that squeezes out and unwashed wet pulp.
Taking formic acid be organic solvent 1., first time pulp washing is carried out under temperature 90 DEG C of environment, with the abundant washing pulp of the form of multistage counter current, obtain scrub raffinate 1., the cooking waste liquor mixing that 1. scrub raffinate squeezes out with above-mentioned, then 80 DEG C, evaporation concentration under the negative pressure of 0.1MPPa, obtains being rich in residue and the phlegma of organism, phlegma is formic acid, can directly reaction medium as slurrying use. Paper pulp after first time washing is that 2. organic solvent carries out second time washing under 70 DEG C of conditions taking ethanol, with the abundant washing pulp of the form of multistage counter current, obtains scrub raffinate 2.. Paper pulp after second time washing is that 3. organic solvent carries out third time washing under 50 DEG C of conditions taking methyl alcohol, with the abundant washing pulp of the form of multistage counter current, obtains scrub raffinate 3.. Paper pulp after third time washing evaporate at 60 DEG C, obtains dry paper pulp and phlegma, phlegma and scrub raffinate 2., 3. mix, rectifying separation recovery organic solvent 2., organic solvent 3. with the cooking reaction medium of minute quantity.
Claims (10)
1. the washing of organic solvent method paper pulp and a method for recovering solvents, comprises step as follows:
By organic solvent pulping gained paper pulp through one or more organic solvent washings, then evaporation drying by the organic solvent evaporation in paper pulp out, obtains dry pulp, and organic vapor is through condensation recycling.
2. the washing of organic solvent method paper pulp according to claim 1 and method for recovering solvents, it is characterised in that, described organic solvent is that methyl alcohol, ethanol, phenol, ether, butanols, ethylene glycol, acetone, formic acid, acetic acid are or/and ethyl acetate.
3. the washing of organic solvent method paper pulp according to claim 1 and method for recovering solvents, it is characterised in that, the washing times of paper pulp is more than twice.
4. the washing of organic solvent method paper pulp according to claim 3 and method for recovering solvents, it is characterised in that, it is identical with organic solvent pulping solvent for use composition that first time washs organic solvent used.
5. the washing of organic solvent method paper pulp according to claim 3 and method for recovering solvents, it is characterised in that, the organic solvent that rear once washing is used and front once washing organic solvent used are mutually miscible; Preferably, compared with the organic solvent that rear once washing organic solvent used is used with front once washing, there is lower boiling point and the latent heat of vaporization.
6. the washing of organic solvent method paper pulp according to claim 1 and method for recovering solvents, it is characterised in that, the boiling point of the temperature≤organic solvent of washing.
7. the washing of organic solvent method paper pulp according to claim 1 and method for recovering solvents, it is characterised in that, first carry out squeezing or taking out filter or centrifugal treating before organic solvent pulping gained pulp washing and before/evaporation drying, to improve the mass dryness fraction of paper pulp.
8. the washing of organic solvent method paper pulp according to claim 1 and method for recovering solvents, it is characterised in that, the washing of described paper pulp, all adopts multistage counter current mode of washing.
9. the washing of organic solvent method paper pulp according to claim 1 and method for recovering solvents, it is characterised in that, evaporation drying, carries out under barometric point or condition of negative pressure; Preferably, evaporation drying temperature is lower than the boiling point of organic solvent.
10. the washing of organic solvent method paper pulp according to claim 1 and method for recovering solvents, it is characterized in that, scrub raffinate after washing and organic vapor by the mode of rectifying, isolate the soluble substance in pulping process reaction medium used, washing process organic solvent used and scrub raffinate through condensed phlegma.
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| CN201610144380.5A CN105672016B (en) | 2016-03-14 | 2016-03-14 | A kind of washing of organic solvent method paper pulp and method for recovering solvents |
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| CN201610144380.5A CN105672016B (en) | 2016-03-14 | 2016-03-14 | A kind of washing of organic solvent method paper pulp and method for recovering solvents |
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| CN105672016A true CN105672016A (en) | 2016-06-15 |
| CN105672016B CN105672016B (en) | 2018-03-30 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109957983A (en) * | 2017-11-08 | 2019-07-02 | 地球循环株式会社 | Cellulose separation method |
| CN111850701A (en) * | 2020-07-29 | 2020-10-30 | 湖南国麻新材料科技有限责任公司 | Degumming method for ramie |
| CN113564955A (en) * | 2020-04-28 | 2021-10-29 | 广州楹鼎生物科技有限公司 | Method for treating plant fiber raw material by acetic acid solution |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281074A (en) * | 1999-07-19 | 2001-01-24 | 西北轻工业学院 | Diwei self-catalyzing alcohol process for pulping |
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2016
- 2016-03-14 CN CN201610144380.5A patent/CN105672016B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281074A (en) * | 1999-07-19 | 2001-01-24 | 西北轻工业学院 | Diwei self-catalyzing alcohol process for pulping |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109957983A (en) * | 2017-11-08 | 2019-07-02 | 地球循环株式会社 | Cellulose separation method |
| CN109957983B (en) * | 2017-11-08 | 2023-08-08 | 地球循环株式会社 | Cellulose separation process |
| CN113564955A (en) * | 2020-04-28 | 2021-10-29 | 广州楹鼎生物科技有限公司 | Method for treating plant fiber raw material by acetic acid solution |
| CN113564955B (en) * | 2020-04-28 | 2023-04-21 | 广州楹鼎生物科技有限公司 | Method for treating plant fiber raw material by acetic acid solution |
| CN111850701A (en) * | 2020-07-29 | 2020-10-30 | 湖南国麻新材料科技有限责任公司 | Degumming method for ramie |
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| CN105672016B (en) | 2018-03-30 |
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Inventor after: Shao Zhiyong Inventor after: Wang Zhaojiang Inventor after: Qin Menghua Inventor before: Wang Zhaojiang Inventor before: Qin Menghua Inventor before: Zhang Yongchao |
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Effective date of registration: 20200927 Address after: 250353 Ji'nan University, Changqing, Shandong Road, No. 3501 Patentee after: Qilu University of Technology Patentee after: MAIYUE Wenbao (Shandong) Technology Development Co.,Ltd. Address before: 250353 Ji'nan University, Changqing, Shandong Road, No. 3501 Patentee before: Qilu University of Technology |
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Address after: 250353 University Road, Changqing District, Ji'nan, Shandong Province, No. 3501 Patentee after: Qilu University of Technology Patentee after: Shandong MAIYUE Wenbao Technology Co.,Ltd. Address before: 250353 University Road, Changqing District, Ji'nan, Shandong Province, No. 3501 Patentee before: Qilu University of Technology Patentee before: MAIYUE Wenbao (Shandong) Technology Development Co.,Ltd. |