CN105200834A - Method of producing pulp by instant vaporization expansion-infiltration in straw sheets - Google Patents
Method of producing pulp by instant vaporization expansion-infiltration in straw sheets Download PDFInfo
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- CN105200834A CN105200834A CN201510637945.9A CN201510637945A CN105200834A CN 105200834 A CN105200834 A CN 105200834A CN 201510637945 A CN201510637945 A CN 201510637945A CN 105200834 A CN105200834 A CN 105200834A
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Abstract
The invention discloses a method of producing pulp by instant vaporization expansion-infiltration in straw sheets. The method includes the steps of adding straw sheets as a raw material into an organic solvent having a boiling point lower than 100 DEG C, according to a straw sheet to organic solvent weight ratio: 1:1 to 1:4 so as to infiltrate the straw sheets for 5-120 min, adding the straw sheets into 100 DEG C boiling water or vapor having a temperature higher than the boiling point of the organic solvent, according to a straw sheet to water weight ratio: 1:1 to 1:20, and producing pulp by boiling under supercritical CO2. cell membranes are caused to expand and break by instant vaporization of the organic solvent among fiber cells of the straw sheets, so that the speed of the removal of intercellular lignin from the straw sheets by boiling is increased by 1 to 5 times, and the usage of the organic solvent is decreased by 2 to 10 times.
Description
Technical field
The present invention relates to a kind of paper-making pulping process, particularly pulping process expand-is permeated in the inner instant vaporization of a kind of blade.
Background technology
Whole world paper and paperboard total output is about 400,000,000 tons/year, and the paper and paperboard output of China ranks first place, the whole world.Paper and paperboard is with slurrying for main manufacture forms, and pulping process can be divided into: chemical method and Mechanical Method, and is in chemical mechanical pulping, semichemical method between the two.The current most of paper mill of China adopts chemical soda pulping process, although the technology of traditional pulping process is very ripe, but the paper pulp often producing 1 ton approximately will discharge 10 tons of black liquor, not only causes the waste of plant resources also easily to cause serious problem of environmental pollution.Therefore the transform and innovation of paper-making pulping process technology did not also stop a moment, and the real motive promoting slurrying scientific technological advance is energy-saving and emission-reduction and environmental protection.
CN201110339908.1 relates to a kind of clean pulping process of high white degree ﹑ high strength chemistry straw pulp, and step is: in grass as raw material, add water, NaOH, hydrogen peroxide and metal ion chelation agent, and 70 DEG C of-80 DEG C of insulations obtain cooking liquor; In cooking liquor, add water, NaOH, hydrogen peroxide and metal ion chelation agent, be incubated second step boiling at 90 DEG C-95 DEG C, screening the pulp, making beating both obtained.
CN201310015474.9 adopts the sodium hydroxide wheat straw normal-pressure pulping process of microwave, and step is as follows: 1) dried wheat straw is put into container, adds after sodium hydroxide solution stirs and obtains mixture; 2) said vesse is moved in micro-wave oven, reflux installed by container, utilize microwave to mixture heating and carry out back flow reaction at ambient pressure, obtaining slurries; 3) slurries are taken out from container, naturally filter black liquor after cooling, handsheet after washing.
CN201410096857.8 discloses a kind of big dragon bamboo pre-preg diethanol amine-anthraquinone pulping by cooking method: adopt Yunnan characteristic assortment big dragon bamboo, use diethanol amine solvent and anthraquinone auxiliary agent pulping by cooking after pre-preg; The paper pulp tool yield obtained by the inventive method is high, and viscosity is higher, the good feature of intensity, and the waste liquid after being separated can directly recycle as pre-preg solution and boiling solvent.
In above-mentioned prior art, although have good slurrying rate, but, the feed hydrogen sodium oxide molybdena etc. adopted has greater environmental impacts, and for the waste water after slurrying be still adopt traditional mode process or larger energy need be expended, fund go process, both increased the funds of business processes waste water on the one hand, easy contaminated environment is not good in process on the other hand.Therefore, need that a kind of slurrying rate is high, technological operation is simple and direct, the pulping process of environmental protection badly.
The information being disclosed in this background technology part is only intended to increase the understanding to general background of the present invention, and should not be regarded as admitting or imply in any form that this information structure has been prior art that persons skilled in the art are known.
Summary of the invention
The present invention is directed to the deficiency that said method exists, provide the method that slurrying expand-is permeated in the inner instant vaporization of a kind of blade.The method technique is simple and direct, easy to operate, utilizes organic solvent to recycle through distillation, decreases the discharge of heavily contaminated waste water, realize cleaner production and the energy-saving and emission-reduction of pulping process.
Blade described in the present invention is the non-wood fibrous raw material described in paper-making pulping process.
For achieving the above object, technical scheme provided by the invention is as follows:
Pulping process expand-is permeated in the inner instant vaporization of blade, step is: be raw material with blade, and add boiling point and infiltrate blade lower than the organic solvent of 100 DEG C, infiltrating time is 5 ~ 120min, add 100 DEG C of boiling water or the temperature water vapour higher than organic solvent boiling point again, then at supercritical CO
2pulping by cooking is carried out under condition.
Pulping process expand-is permeated in the inner instant vaporization of blade, and its more detailed step is:
(1) with blade non-wood-fiber for digester put into by raw material, add boiling point lower than 100 DEG C organic solvent infiltrate blade, infiltrating time is 5 ~ 120min, then add 100 DEG C of boiling water or or temperature make the organic solvent instant vaporization expansion damage cell membrane of blade fibrous inside higher than the steam of the organic solvent boiling point added, accelerate organic solvent, surfactant etc. and permeate and enter blade fibrocyte interbed, cell membrane and cell angle thus reach the object of the lignin removed in blade;
(2) CO is passed into
2gas, and raise digester temperature and pressure to supercritical CO
2carry out the pulping by cooking of blade raw material under state, utilize organic solvent and supercritical CO
2carry out self-catalysis and remove lignin between blade fibrocyte.In course of reaction, organic solvent forms the steam etc. of steam and period generation, utilizes supercritical CO
2, organic vapor and water vapour be entrained with the degradation product removing lignin and constantly flow out digester, obtain degradation solution, realize the lignin degradation reaction-separation coupling between blade fibrocyte.
The slurry that blade boiling terminates and degradation solution put into jet discharging device, spurt slurry and degradation solution, then obtain slurry and reducing sugar through separating-purifying.
As further restriction, described blade is the one in bamboo, straw, straw, reed, bagasse, cotton stalk, cornstalk.
As further restriction, the blade added and organic solvent mass ratio are 1:1 ~ 1:4.
As further restriction, the amount of the 100 DEG C of boiling water added is according to the organic solvent added: the boiling water mass ratio added is that 1:1 ~ 1:20 adds.
As further restriction, the amount of the steam added is according to the organic solvent added: the mass ratio of the steam added is that 1:1 ~ 1:10 adds.
As further restriction, add surfactant when adding boiling water or steam simultaneously, add after mixing by surfactant with boiling water or steam simultaneously, the amount adding surfactant accounts for 0.004 ~ 0.01% of the blade quality added.
As further restriction, at supercritical CO
2under condition, the condition of pulping by cooking is: supercritical CO
2pressure be 7.1 ~ 20.0MPa, temperature is 80 ~ 300 DEG C, and digestion time is 0.5 ~ 3.0h.
As further restriction, the flow adding 100 DEG C of boiling water is 1 ~ 5 times of kg/min of the amount of organic solvent for infiltrating blade, namely per minutely passes into 1 ~ 5 times for infiltrating 100 DEG C of boiling water of the organic solvent amount of blade.
As further restriction, the temperature added is the amount kg/min of the organic solvent that 0.3 ~ 2 times adds higher than the flow of the water vapour of organic solvent boiling point, namely per minutely passes into 0.3 ~ 2 times for infiltrating 100 DEG C of steam of the organic solvent amount of blade.
As further restriction, described organic solvent is at least one in ether, methyl tertiary butyl ether(MTBE), ethyl tert-butyl ether (ETBE), methyl alcohol, ethanol, furans, oxolane, methyl formate, Ethyl formate, methyl acetate, ethyl acetate, dimethyl carbonate, vinylacetate, butane, pentane, hexane, cyclohexane, benzinum, and namely boiling point is lower than the organic solvent of less than 100 DEG C.
As further restriction, described surfactant is fatty alcohol polyethenoxy ether class (AEO), breast lark A, Emulsifier MOA, peregal, polyoxyethylene carboxylate, alkylphenol polyoxyethylene (TX-10, OP-10), sapn (span), tween (Tween) 60-100, lauryl sodium sulfate, sodium methylene bis-naphthalene sulfonate (NNO), Dodecyl Polyoxyethylene Ether, dodecane amido propionic acid, empgen BB, alkylsulfonate (AS), sodium cetanesulfonate (SAS), at least one in petroleum sodium sulfonate (PS).
Compared with prior art, the present invention has following beneficial effect:
1, the inventive method causes cell membrane swelling fracture by organic solvent fast vaporizing between blade fibrocyte, and the speed making blade boiling remove iuntercellular lignin accelerates 1 ~ 5 times, and the consumption of organic solvent reduces 2 ~ 10 times;
2, with supercritical CO
2be dissolved in Bronsted acid that water formed, organic solvent and surfactant remove lignin in blade, wherein organic solvent recycles through distillation, decrease the discharge of heavily contaminated waste water, particularly most of China paper mill adopts alkaline process chemical pulping, often produce 1 ton of paper pulp and will discharge 10 tons of black liquor, and pulping process of the present invention is without black liquor also non-exhaust emission, it is a kind of pulping process of environmental protection;
3, the method for digester vapour phase flowing is adopted to make the blade iuntercellular lignin degradation product of generation constantly leave reacting environment, realize the lignin degradation reaction-separation coupling between blade fibrocyte, the feedback inhibition that elimination catabolite adds up and causes, improve reaction rate and the equilibrium conversion of the poly pentose degraded in blade lignin and blade, improve 1 ~ 5 times;
4, the inventive method exceeds 5% ~ 10% than the slurry total yield of traditional pulping process, and gained slurry hardness is low, intensity is large, whiteness is high, bleachability is good.
Detailed description of the invention
Be described in detail below in conjunction with detailed description of the invention, but be to be understood that protection scope of the present invention not by the restriction of detailed description of the invention.
Embodiment 1:
Take blade: i.e. bagasse 100kg; Organic solvent 100kg.The surfactant peregal of the bagasse quality 0.004% added, 100 DEG C of boiling water 100kg, put into boiling water by peregal and mix, for subsequent use.Blade bagasse is added in digester, add the above-mentioned ethanol Homogeneous phase mixing taken again and infiltrate bagasse, infiltrating time is 10min, then the above-mentioned 100 DEG C of boiling water having added surfactant are added, boiling water flow is 100kg/min, make to penetrate into sugarcane fibre intercellular ethanol instant vaporization expansion damage cell membrane, then in digester, pass into CO
2, control reaction pressure 7.1MPa, reaction temperature 80 DEG C, reaction time 0.5h, utilizes organic solvent ethanol, surfactant peregal and supercritical CO
2carry out self-catalysis and remove lignin between blade fibrocyte.In course of reaction, ethanol forms the steam etc. of steam and period generation, i.e. period, utilize supercritical CO
2, organic vapor and water vapour be entrained with the degradation product removing lignin and constantly flow out digester, obtain degradation solution, realize the lignin degradation reaction-separation coupling between blade fibrocyte.Spurt slurry and degradation solution after boiling terminates, separating-purifying, pulp yield is 66.4%, and Reducing sugar is 10.2%.
Embodiment 2
By the method step repeating embodiment 1 with each component of specifying in following table 1 and each technological parameter.
Embodiment 3
By the method step repeating embodiment 1 with each component of specifying in following table 1 and each technological parameter.
Embodiment 4
By the method step repeating embodiment 1 with each component of specifying in following table 1 and each technological parameter.
Embodiment 5
By the method step repeating embodiment 1 with each component of specifying in following table 1 and each technological parameter.
Embodiment 6
By the method step repeating embodiment 1 with each component of specifying in following table 1 and each technological parameter.
Embodiment 7
By the method step repeating embodiment 1 with each component of specifying in following table 1 and each technological parameter.
Embodiment 8
By the method step repeating embodiment 1 with each component of specifying in following table 1 and each technological parameter.
Embodiment 9
By the method step repeating embodiment 1 with each component of specifying in following table 1 and each technological parameter.
Table 1
In table 1,100 DEG C of boiling water and steam capable, "------" symbol represents that this material does not add in this embodiment.
The aforementioned description to concrete exemplary of the present invention is to illustrate and the object of illustration.These descriptions not want the present invention to be defined as disclosed precise forms, and obviously, according to above-mentioned instruction, can much change and change.The object selected exemplary embodiment and describe is to explain certain principles of the present invention and practical application thereof, thus those skilled in the art can be realized and utilize various different exemplary of the present invention and various different selection and change.Scope of the present invention is intended to limited by claims and equivalents thereof.
Claims (9)
1. the inner instant vaporization of a blade is expanded-permeates pulping process, it is characterized in that, step is: take blade as raw material, add boiling point lower than 100 DEG C organic solvent infiltrate blade, infiltrating time is 5 ~ 120min, add 100 DEG C of boiling water or the temperature water vapour higher than organic solvent boiling point again, then at supercritical CO
2pulping by cooking is carried out under condition.
2. the inner instant vaporization of blade is expanded-permeates pulping process according to claim 1, it is characterized in that: described blade is the one in bamboo, straw, straw, reed, bagasse, cotton stalk, cornstalk.
3. the inner instant vaporization of blade is expanded-permeates pulping process according to claim 1, it is characterized in that: the blade added and organic solvent mass ratio are 1:1 ~ 1:4.
4. the inner instant vaporization of blade is expanded-permeates pulping process according to claim 1, it is characterized in that: the amount of the 100 DEG C of boiling water added is according to the organic solvent added: the boiling water mass ratio added is that 1:1 ~ 1:20 adds.
5. the inner instant vaporization of blade is expanded-permeates pulping process according to claim 1, and it is characterized in that, the amount of the steam added is according to the organic solvent added: the mass ratio of the steam added is that 1:1 ~ 1:10 adds.
6. the inner instant vaporization of blade is expanded-permeates pulping process according to claim 1, it is characterized in that: when adding boiling water or steam, add surfactant simultaneously, add after mixing with boiling water or steam by surfactant, the amount adding surfactant accounts for 0.004 ~ 0.01% of the blade quality added simultaneously.
7. the inner instant vaporization of blade is expanded-permeates pulping process according to claim 1, it is characterized in that, at supercritical CO
2under condition, the condition of pulping by cooking is: supercritical CO
2pressure be 7.1 ~ 20.0MPa, temperature is 80 ~ 300 DEG C, and digestion time is 0.5 ~ 3.0h.
8. the inner instant vaporization of blade is expanded-permeates pulping process according to claim 1, it is characterized in that: the flow adding 100 DEG C of boiling water is 1 ~ 5 times of kg/min of the amount of organic solvent for infiltrating blade.
9. the inner instant vaporization of blade is expanded-permeates pulping process according to claim 1, it is characterized in that: the temperature added is the amount kg/min of the organic solvent that 0.3 ~ 2 times adds higher than the flow of the water vapour of organic solvent boiling point.
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| CN201510637945.9A CN105200834B (en) | 2015-09-30 | 2015-09-30 | Pulping process expand-is permeated in instant vaporization inside blade |
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| CN201510637945.9A CN105200834B (en) | 2015-09-30 | 2015-09-30 | Pulping process expand-is permeated in instant vaporization inside blade |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1552993A (en) * | 2003-05-29 | 2004-12-08 | 中国科学院成都有机化学研究所 | Cooking catalyst for papermaking and pulping |
| US20130017579A1 (en) * | 2010-03-30 | 2013-01-17 | Cornell University | Biphasic supercritical carbon dioxide-water pretreatment of lignocellulosic biomass |
| CN104674585A (en) * | 2015-02-15 | 2015-06-03 | 广西大学 | Method and device for hydrolyzing pulping |
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2015
- 2015-09-30 CN CN201510637945.9A patent/CN105200834B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1552993A (en) * | 2003-05-29 | 2004-12-08 | 中国科学院成都有机化学研究所 | Cooking catalyst for papermaking and pulping |
| US20130017579A1 (en) * | 2010-03-30 | 2013-01-17 | Cornell University | Biphasic supercritical carbon dioxide-water pretreatment of lignocellulosic biomass |
| CN104674585A (en) * | 2015-02-15 | 2015-06-03 | 广西大学 | Method and device for hydrolyzing pulping |
Non-Patent Citations (1)
| Title |
|---|
| DANIEL PASQUINI等: "Extraction of lignin from sugar cane bagasse and Pinus taeda wood chips using ethanol–water mixtures and carbon dioxide at high pressures", 《SUPERCRITICAL FLUIDS》 * |
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