CN105525389B - The zero-emission recovery process of Pulp Fibers element alkali pressed liquor - Google Patents
The zero-emission recovery process of Pulp Fibers element alkali pressed liquor Download PDFInfo
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Abstract
A kind of zero-emission recovery process of Pulp Fibers element alkali pressed liquor mainly includes level-one UF membrane, second level UF membrane, hemicellulose precipitations, three-level UF membrane, hemicellulose recycle and level Four UF membrane.The present invention is by alkali pressed liquor integrated treatment, not only recycle alkali, hemicellulose and oligosaccharide are recycled simultaneously, the whole of waste resource are realized to recycle, solves the recycling problem of hemicellulose, expand raw material sources for chemical fibre factory, reduce production cost, lowers environmental pollution and provide effective solution method.
Description
Technical field
The present invention relates to three-protection design more particularly to a kind of zero-emission recovery process of Pulp Fibers element alkali pressed liquor.
Background technique
It take chemical pulp (plant celluloses such as wood pulp or cotton pulp, straw pulp, bamboo pulp, reed pulp) as the viscose rayon (people of raw material
Make silk) production in during, cellulose alkali liquor treating process be manufacture viscose rayon the first step.The manufacture of usual fiber product
It is required that the chemical cellulose purity as raw material reaches 92% or more (not less than 90%).Since its raw material still contains more half
Cellulose, therefore must will be dissolved out hemicellulose with aqueous slkali in impregnation technology, high-intensitive cellulose could be obtained.
Hemicellulose concentration is high, and extremely disadvantageous influence will be generated to cellulose viscose manufacturing technique and final product quality.
Main component in alkali pressed liquor is sodium hydroxide and hemicellulose.The processing of existing press lye mostly uses nanofiltration
Technology therefrom separates hemicellulose, obtains more pure lye.Lye by purification can be with direct reuse to work
In skill.But part alkali is only realized reuse by nanofiltration membrane.Hemicellulose in its trapped fluid is concentrated, and is still contained in concentrate
There is a large amount of alkali.For the part feed liquid as salkali waste for neutralizing, hemicellulose enters wastewater treatment at present.Or it is recycled using calcination
Caustic soda, hemicellulose is burned, and hemicellulose is underutilized in above-mentioned technique.
Summary of the invention
The purpose of the present invention provides a kind of Pulp Fibers element exactly in order to solve the above-mentioned problems of the prior art
The zero-emission recovery process of alkali pressed liquor.
In order to achieve the above object, the invention adopts the following technical scheme: a kind of Pulp Fibers element alkali pressed liquor
Zero-emission recovery process, which is characterized in that mainly comprise the steps that
A, level-one UF membrane
Alkali pressed liquor is sent into level-one film separation system, hemicellulose is trapped to form level-one film concentrate, and level-one film is saturating
The lye that liquid is purifying is crossed, it can direct reuse；
B, second level UF membrane
Level-one film concentrate obtained by step A is sent into second level film separation system, hemicellulose is further concentrated, and obtains two
Grade film concentrate contains oligosaccharide and alkali into step C processing in secondary membrane permeate, to be processed；
C, hemicellulose acidolysis
Secondary membrane concentrate obtained by step B carries out acidolysis by one of following two methods:
C1, acid is added in secondary membrane concentrate, until acid content reaches 0.2-1.0% in system, is heated to >=100 DEG C,
Laser heating 1-4 hours, xylose hydrolysis fluid is obtained, using neutralization, active carbon decoloring, ion exchange, concentration, crystallization, is obtained
Crystalline xylose；
C2, acid is added in secondary membrane concentrate, is adjusted to pH < 7, obtains suspension, gained suspension is sent into three-level
Film separation system obtains three-level film concentrate, and further acid adding acid content into liquid reaches in gained three-level film concentrate
0.2-1.0% is heated to >=100 DEG C, laser heating 1-4 hours, obtains xylose hydrolysis fluid, using neutralize, active carbon decoloring,
Ion exchange, concentration, crystallization, obtain crystalline xylose；Contain oligosaccharide and alkali in three-level film permeate, it is to be processed.
Further include step D: sending secondary membrane permeate obtained by step B or with three-level film permeate obtained by step C2 into level Four
Film separation system obtains the lye that level Four film permeate is purifying, can direct reuse；During the level Four film concentrate being trapped passes through
With concentration, decoloration, desalting processing, oligosaccharide solution is obtained, for recycling oligosaccharide.
The level-one film separation system uses nanofiltration membrane, and the molecular weight that shuts off is 100-5000, or retains to sodium chloride
Rate is lower than 90% or pore size filter 1-10nm, and at 10-80 DEG C, operating pressure is controlled in 1-5Mpa for operation temperature control.
For the second level film separation system using tubular type or board-like nanofiltration membrane or ultrafiltration membrane, the molecular weight that shuts off is 100-
5000 or pore size filter 1-10nm, using cross-flow filtration form, film surface flow control is in 1-6 meter per second, operation temperature control
At 10-80 DEG C, operating pressure is controlled in 0.1-4MPa system.
For the three-level film separation system using tubular type or board-like nanofiltration membrane or ultrafiltration membrane, the molecular weight that shuts off is 200-
100000 or membrane aperture less than 0.2 micron, using cross-flow filtration form, film surface flow control is in 1-6 meter per second, operation temperature
At 10-80 DEG C, operating pressure is controlled in 0.1-4MPa for degree control.
The level Four film separation system uses nanofiltration membrane, and the molecular weight that shuts off is 100-1000, or cuts to sodium chloride
Stay rate lower than 90%, at 30-60 DEG C, operating pressure is controlled in 1-5Mpa for operation temperature control.
For 200-400, operation temperature is controlled in 50- the molecular weight that shuts off for the nanofiltration membrane that the level-one film separation system uses
60 DEG C, operating pressure is controlled in 2-4Mpa.
The molecular weight that shuts off of nanofiltration membrane or ultrafiltration membrane that the second level film separation system uses is 500-5000, operation temperature
Control is at 50-60 DEG C.
For 100-400, operation temperature is controlled in 50- the molecular weight that shuts off for the nanofiltration membrane that the level Four film separation system uses
60 DEG C, operating pressure is controlled in 2-4Mpa.The pH value that the nanofiltration membrane that the level Four film separation system uses can be resistant to is greater than 11.
Add water dialysis respectively in the concentration process of level-one film separation system and second level film separation system.
Acid, including sulfuric acid, hydrochloric acid, oxalic acid, citric acid, acetic acid used in the step C etc..
The nanofiltration membrane or ultrafiltration membrane that above-mentioned level-one film separation system, second level film separation system and three-level film separation system use
For polymer material film or inorganic material film, the high molecular material is selected from polyether sulfone, polysulfones, armaticity polysulfones, polyvinylidene fluoride
The mixture of one or more of alkene, polyvinyl chloride, polyketone, polyether-ketone, polytetrafluoroethylene (PTFE), polyethylene or polyamide；It is described
Inorganic material is selected from one of aluminum oxide, zirconium dioxide, titanium dioxide, stainless steel, alloy, nickel alloy or silicon carbide.
The nanofiltration membrane that above-mentioned level Four film separation system uses be by polyether sulfone, polysulfones, armaticity polysulfones, Kynoar,
Volume made of the mixture of one or more of polyvinyl chloride, polyketone, polyether-ketone, polytetrafluoroethylene (PTFE), polyethylene or polyamide
Formula nanofiltration membrane or hollow fiber nanofiltration membrane, the pH value that can be resistant to are greater than 11.
The level-one film separation system includes a nano-filtration unit and at least one pretreatment unit, and alkali pressed liquor first passes through pre-
Nano-filtration unit, pretreatment unit belt filter, bag filter or automatic cleaning filtering are entered back into after processing unit processes
Device is filtered alkali pressed liquor, and filter screen aperture is 1-100 microns.
It is real the present invention provides recycle-water, xylo-oligosaccharide, hemicellulose and alkali in a kind of new chemically slurry alkali pressed liquor
The technique of existing zero-emission.Whole compared with prior art is using nanofiltration system recycling alkali technique, in the present invention in alkali pressed liquor
Alkali can recycle in the different workshop sections of viscose production.Whole recycling of xylo-oligosaccharide and hemicellulose, alkali are obtained simultaneously
The rate of recovery is close to 100%.The separation of oligosaccharide not only can be obtained high-value product, while reduce and apply rear hemicellulose in lye
In accumulation, significantly more efficient guarantee product quality.The present invention realizes the whole of waste resource and recycles, and solves half fiber
The recycling problem of element is tieed up, expands raw material sources for chemical fibre factory, reduces production cost, lowers environmental pollution and provides effective solution
Certainly method.For using the high plant production viscoses of xylans content such as broadleaf or bagasse can using present invention process
To obtain xylose and xylo-oligosaccharide product.
The processing recovery process of Pulp Fibers element alkali pressed liquor of the invention has the advantages that following significant and feature:
1, entire technique realizes zero-emission；
2, the recycling of hemicellulose is realized；
3, it realizes the separation of oligosaccharide and hemicellulose, can get the byproduct of higher value；
4, the rate of recovery of lye is improved.
Specific embodiment
In alkali pressed liquor in the present invention, the concentration of alkali is 10-30%, hemicellulose level 15-60g/L.
The raw material sources of dipping can be fine for timber, cotton, straw, sugarcane, bamboo, reed, the stem containing fiber, leaf
Dimension or said mixture.It is preferred that wood pulp pulp is as cellulose origin.Wood pulp source includes cork, hardwood.Half fiber in cellulose
Content can reach 30%.
Maceration extract after alkali process obtains press lye after plate compression.Its naoh concentration usually exists
Between 150-300g/L, half fiber content is according to raw material difference is different and the accumulation of system hemicellulose, usually in 15-
Between 60g/L.It is pumped up into level-one film separation system.The pore size filter of level-one film shuts off molecular weight 100-5000, or to chlorine
Change sodium rejection and is lower than 90% or pore size filter 1-10nm.In operating pressure 0.1-5MPa, 10-80 DEG C of temperature is operated, preferably
2.5-4MPa, 50-60 DEG C of operations, sodium hydroxide and water penetrate film, and hemicellulose is rejected by concentration.Usual hemicellulose concentration
To 50-100g/L, the content 1-10g/L of hemicellulose, alkali concentration are identical as feeding liquid in permeate.Permeate is placed in storage tank
It is spare, it can be directly used for impregnation technology.The concentrate of level-one film separation system is sent into second level film separation system and continues to be concentrated at this time.
Level-one film separation system alkali recovery is usually in 50-75%.Or level-one film is concentrated to 50-100g/L, continues plus water is dialysed, make
Alkali in concentrate reduces as far as possible, adds water to hemicellulose concentration 50-100g/L in concentrate, stops dialysis, and concentrate is sent into
Second level film separation system.
By the hemicellulose concentrate of level-one film separation system initial concentration, it is pumped up into second level film separation system.Film
Shut off molecular weight be 100-5000 or pore size filter 1-10nm.In operating pressure 0.1-4MPa, 10-80 DEG C of temperature is operated,
It is preferred that 0.25-0.7MPa, 50-60 DEG C of operations, add water to dialyse, sodium hydroxide and water penetrate film, and hemicellulose is rejected by.Add water
Naoh concentration 10g/L is dialysed into concentrate hereinafter, concentrate is stand-by.By the processing of second level film separation system, half fiber
Dimension element is further concentrated, and hemicellulose concentration can reach 100-200g/L in concentrate.
Acid is added in secondary membrane concentrate, until acid content reaches 0.2-2.0% in system, is heated to 100-130 degrees Celsius,
1-4 hours, hydrolysis obtained xylose hydrolysis fluid.By neutralizing, active carbon decoloring, ion exchange is concentrated, crystallization, obtains crystallization wood
Sugar.
A kind of method for preparing xylose of optimization is the concentrate of secondary membrane, and the concentrate of second level film separation system is placed in
In tank, it is slowly added to inorganic acid, such as sulfuric acid, nitric acid, hydrochloric acid, citric acid, phosphoric acid.With pH value be stepped down to 7 hereinafter,
It is preferred that pH5-6.Hemicellulose is precipitated.Obtain the suspension of hemicellulose.The suspension enters three-level film separation system.Three-level film
The molecular weight that shuts off be 200-100000 or membrane aperture less than 0.2 micron.In operating pressure 0.1-4MPa, 10-80 DEG C of temperature
Operation, preferably 0.25-0.7MPa, 30-60 DEG C of operation, salt and water penetrate film, and hemicellulose is rejected by concentration.It is added a certain amount of
Water-dialyzing concentrated solution for washing, enable the salt at concentrate end through film, hemicellulose is further purified.It is concentrated in dialysis.It is dense
Hemicellulose concentration is up to 20-30% in contracting liquid.The concentration liquid suspensions hydrolysis prepares xylose.Hemicellulose concentration improves, and
And by purification, further acid adding acid content 0.2-2.0% into liquid, 100-125 degrees Celsius of temperature holding, holding 1-4 is small
When.Obtain xylose hydrolysis fluid.Neutralized, active carbon decoloring is concentrated, and crystallization obtains crystalline xylose.The permeate of three-level membranous system
In containing oligosaccharide and salt enter the processing of level Four membranous system.
Contain oligosaccharide, concentration 1-70g/L in secondary membrane permeate.Secondary membrane permeate can enter level Four UF membrane system
The molecular weight that shuts off of system processing, film is 100-1000, or is lower than 90% to sodium chloride rejection.Oligosaccharide is concentrated,
Alkali and water penetrate film.1% or less naoh concentration in the permeate.For the ingredient of each technique in viscose glue production process, wash
Water etc..Obtained concentration of oligosaccharide reaches 20-30%.Concentrate obtains oligosaccharide syrup through techniques such as decoloration, ion-exchange, concentrations.
Embodiment 1:
100 cubic metres of alkali pressed liquor, naoh concentration is 220g/L, hemicellulose level 35g/L in charging.In temperature
It spends 50 degrees Celsius and enters level-one film separation system, the molecular weight 200 that shuts off of film.It is operated at pressure 2-3MPa.When being concentrated to half
When cellulose cellulose content 40-70g/L, concentrate, which enters second level film separation system, to be continued to dialyse, concentration.The molecule that shuts off of secondary membrane
Amount 1000.At 50 degrees Celsius, operated under the conditions of 0.5MPa.Alkali concentration 5-10g/L in concentrate is carried out dialysis, hemicellulose is concentrated to
40-100g/L, the concentrate are spare.
Above-mentioned secondary membrane concentrate, is placed in reactor tank, and sulfuric acid is added, and neutralizes in concentrate after residual alkali, then is extremely concentrated
Acid content reaches 0.5% in liquid, is passed through steam to temperature and reaches 120-125 degrees Celsius, and control steam pressure is no more than 0.2Mpa,
Temperature is no more than 125 degrees Celsius, holds time 3 hours.Reaction terminates.Obtain xylose hydrolysis fluid.By neutralizing, active carbon is de-
Color, ion exchange are concentrated, and crystallization obtains crystalline xylose.
Level-one film separation system filter liquor, which is placed in, to be filtered out in flow container, can direct reuse.The filter liquor of second level film separation system
Into level Four film separation system.The molecular weight 200-400 that shuts off of level Four film, operating pressure 2.5MPa, 45 degrees Celsius of temperature, concentration
Oligosaccharide in filter liquor.It is concentrated into 200 grams per liter of oligosaccharide in concentrate.Through desalination, decoloration, using conventional evaporation and concentration, obtain
To the syrup of 60% or more Solid content.Filter liquor contains a small amount of alkali, is back in technique as pure water.
Embodiment 2:
Secondary membrane concentrate obtained in embodiment 1, wherein hemicellulose level 100g/L, naoh concentration 10g/L.
30% hydrochloric acid solution is added in the container for placing above-mentioned concentrate, it is stirring while adding to PH5-6.Hemicellulose is precipitated.Into
Three-level film separation system is separated.The pore size filter of three-level film film is 5-200nm.In 0.6MPa pressure, film surface stream is kept
Fast 5 meter per seconds.Add water to dialyse in concentration, obtains the hemicellulose concentrate that can directly recycle.Hemicellulose concentration 25%.
The hemicellulose concentrate is placed in reactor tank, and hydrochloric acid acid content into concentrate is added to reach 0.2%, is passed through steam to temperature and is reached
To 120-125 degrees Celsius, control steam pressure is no more than 0.2Mpa, and temperature is no more than 125 degrees Celsius, holds time 4 hours.Instead
It should terminate.Obtain xylose hydrolysis fluid.By neutralizing, active carbon decoloring, ion exchange is concentrated, and crystallization obtains crystalline xylose.
Embodiment 3
100 cubic metres of alkali pressed liquor, naoh concentration is 220g/L, hemicellulose level 35g/L in charging.In temperature
It spends 50 degrees Celsius and enters level-one film separation system, the molecular weight 5000 that shuts off of film is operated at pressure 0.2-0.7MPa.Work as concentration
When to hemicellulose cellulose content 40-70g/L, water-dialyzing is added in tank, until alkali concentration 40-100g/L, concentrate enter second level
Film separation system continues to dialyse, concentration.The molecular weight 5000 that shuts off of secondary membrane is grasped under the conditions of 0.2-0.7MPa at 50 degrees Celsius
Make.Alkali concentration 5-10g/L in concentrate is carried out dialysis, hemicellulose is concentrated to 40-100g/L, and the concentrate is spare.
Claims (9)
1. a kind of zero-emission recovery process of Pulp Fibers element alkali pressed liquor, which is characterized in that mainly comprise the steps that
A, level-one UF membrane
Alkali pressed liquor is sent into level-one film separation system, hemicellulose is trapped to form level-one film concentrate, level-one film permeate
It, can direct reuse for the lye of purifying；
B, second level UF membrane
Level-one film concentrate obtained by step A is sent into second level film separation system, hemicellulose is further concentrated, and obtains secondary membrane
Concentrate contains oligosaccharide and alkali into step C processing in secondary membrane permeate, to be processed；
C, hemicellulose acidolysis
Acid is added in secondary membrane concentrate, is adjusted to pH < 7, obtains suspension, gained suspension is sent into three-level UF membrane
System obtains three-level film concentrate, and further acid adding acid content into liquid reaches 0.2- in gained three-level film concentrate
1.0%, >=100 DEG C are heated to, laser heating 1-4 hours, obtains xylose hydrolysis fluid, using neutralization, active carbon decoloring, ion
Exchange, concentration, crystallization, obtain crystalline xylose；Contain oligosaccharide and alkali in three-level film permeate, it is to be processed；
D: three-level film permeate obtained by secondary membrane permeate obtained by step B and step C is sent into level Four film separation system, obtains four
Grade film permeate is the lye of purifying, can direct reuse；The level Four film concentrate being trapped is by neutralizing, being concentrated, decolourize, desalination
Processing, obtains oligosaccharide solution, for recycling oligosaccharide；
The molecular cut off of the level-one film separation system is 200-400,
The molecular cut off of the second level film separation system is 500-5000,
The molecular cut off of the level Four film separation system is 100-400, and the level Four film separation system uses nanofiltration membrane, can
It is greater than 11 with the pH value of tolerance.
2. the zero-emission recovery process of Pulp Fibers element alkali pressed liquor according to claim 1, it is characterised in that: described
Level-one film separation system uses nanofiltration membrane, and at 10-80 DEG C, operating pressure is controlled in 1-5MPa for operation temperature control.
3. the zero-emission recovery process of Pulp Fibers element alkali pressed liquor according to claim 2, it is characterised in that: described
At 50-60 DEG C, operating pressure is controlled in 2-4MPa the control of level-one film separation system operation temperature.
4. the zero-emission recovery process of Pulp Fibers element alkali pressed liquor according to claim 1, it is characterised in that: described
Second level film separation system is using tubular type or board-like nanofiltration membrane or ultrafiltration membrane, using cross-flow filtration form, film surface flow control
In 1-6 meter per second, at 10-80 DEG C, operating pressure is controlled in 0.1-4MPa for operation temperature control.
5. the zero-emission recovery process of Pulp Fibers element alkali pressed liquor according to claim 4, it is characterised in that: described
Second level film separation system operation temperature is controlled at 50-60 DEG C.
6. the zero-emission recovery process of Pulp Fibers element alkali pressed liquor according to claim 1, it is characterised in that: described
Three-level film separation system is using tubular type or board-like nanofiltration membrane or ultrafiltration membrane, molecular cut off 200-100000 or film
Aperture is less than 0.2 micron, and using cross-flow filtration form, film surface flow control is controlled in 1-6 meter per second, operation temperature in 10-80
DEG C, operating pressure is controlled in 0.1-4MPa.
7. the zero-emission recovery process of Pulp Fibers element alkali pressed liquor according to claim 1, it is characterised in that: described
Level Four film separation system use nanofiltration membrane, at 30-60 DEG C, operating pressure is controlled in 1-5MPa for operation temperature control.
8. the zero-emission recovery process of Pulp Fibers element alkali pressed liquor according to claim 7, it is characterised in that: described
At 50-60 DEG C, operating pressure is controlled in 2-4MPa the control of level Four film separation system operation temperature.
9. the zero-emission recovery process of Pulp Fibers element alkali pressed liquor according to claim 1, it is characterised in that: one
Add water dialysis in the concentration process of grade film separation system and second level film separation system respectively.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107724151A (en) * | 2017-09-30 | 2018-02-23 | 山东福田药业有限公司 | A kind of dissolving pulp alkali immersion liquid handling process |
| CN109554948B (en) * | 2018-11-28 | 2021-01-01 | 宜宾丝丽雅股份有限公司 | Multistage alkali liquor recovery process |
| CN111661967A (en) * | 2020-05-21 | 2020-09-15 | 莱特莱德（北京）环境技术股份有限公司 | System and method for recovering alkali in viscose fiber production squeezing waste liquid by using double-membrane method |
| CN111484569A (en) * | 2020-05-29 | 2020-08-04 | 新疆中泰纺织集团有限公司 | Zero-emission treatment method of viscose squeezed alkali liquor |
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|---|---|---|---|---|
| CN1450001A (en) * | 2003-05-15 | 2003-10-22 | 凯能高科技工程（上海）有限公司 | Method for recovering alkali and hemicellulose from chemical fibre waste liquid |
| CN103572635A (en) * | 2013-05-28 | 2014-02-12 | 上海凯鑫分离技术有限公司 | Processing and recovering process of chemical fiber pulp cellulose alkali pressed liquor |
| CN104099431A (en) * | 2014-08-01 | 2014-10-15 | 沈阳新华环境工程有限公司 | Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor |
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2014
- 2014-10-24 CN CN201410579153.6A patent/CN105525389B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1450001A (en) * | 2003-05-15 | 2003-10-22 | 凯能高科技工程（上海）有限公司 | Method for recovering alkali and hemicellulose from chemical fibre waste liquid |
| CN103572635A (en) * | 2013-05-28 | 2014-02-12 | 上海凯鑫分离技术有限公司 | Processing and recovering process of chemical fiber pulp cellulose alkali pressed liquor |
| CN104099431A (en) * | 2014-08-01 | 2014-10-15 | 沈阳新华环境工程有限公司 | Method for extracting xylose from viscoce chemical fiber squeezed alkali liquor |
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Address after: 201206 room 5-16, building 1999, Zhang Heng Road, Shanghai, China (Shanghai) free trade zone, No. 7 Applicant after: SHANGHAI KAIXIN ISOLATION TECHNOLOGY CO., LTD. Address before: 201206 room 5-16, building 1999, Zhang Heng Road, Shanghai, Pudong New Area, China, 7 Applicant before: Shanghai Kai Xin isolation technique company limited |
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Address after: 201210, Shanghai, China (Shanghai) free trade zone, Zhangjiang Road, No. 665, 3, Pudong New Area Applicant after: SHANGHAI KAIXIN ISOLATION TECHNOLOGY CO., LTD. Address before: 201206 room 5-16, building 1999, Zhang Heng Road, Shanghai, China (Shanghai) free trade zone, No. 7 Applicant before: SHANGHAI KAIXIN ISOLATION TECHNOLOGY CO., LTD. |
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