CN101812813A - Method and device for treating paper-making black liquid acid-precipitation waste liquid film - Google Patents

Method and device for treating paper-making black liquid acid-precipitation waste liquid film Download PDF

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Publication number
CN101812813A
CN101812813A CN 201010140224 CN201010140224A CN101812813A CN 101812813 A CN101812813 A CN 101812813A CN 201010140224 CN201010140224 CN 201010140224 CN 201010140224 A CN201010140224 A CN 201010140224A CN 101812813 A CN101812813 A CN 101812813A
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China
Prior art keywords
membrane
waste liquid
reverse osmosis
processing method
film
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CN 201010140224
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Chinese (zh)
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刘久清
陈金山
文飙
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Central South University
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Central South University
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Abstract

The invention relates to a method and a device for treating a paper-making black liquid acid-precipitation waste liquid film, wherein the device comprises an ultrafiltration film, a nanofiltration film and a reverse osmosis film, wherein the films are all macromolecular organic films. The invention also discloses a method for treating the paper-making black liquid acid-precipitation waste liquid film. In the method, waste water passes through the ultrafiltration film, the nanofiltration film and the reverse osmosis film in sequence, and the films can be replaced and cleaned for repeated use. The device has the advantages of waste water discharge reduction, environmental protection and water-resource conservation.

Description

A kind of black liquid acid out waste liquid membrane processing method and device thereof
Technical field
The present invention relates to a kind of acid out of black liquid efficiently waste liquid membrane processing method, particularly a kind of method that makes the part water circulation use.
Background technology
The most paper mills of China are raw material with the non-wood-fiber, mainly constitute with cellulose, lignin and hemicellulose (being the poly-pentose class) three big compositions.Cellulose is the main raw material of papermaking, cellulose belongs to the alkali insoluble matter, in the alkali lye in rotary spherical digester, lignin and hemicellulose are dissolvable in water and form black liquor in the alkali lye, therefore, wheat straw is in the rotary spherical digester digestion process, lignin and hemicellulose are dissolved by aqueous slkali, formation contains water, residual alkali, cellulose, the original slurry of alkali lignin and hemicellulose, original slurry is separated through slurries, the cellulose that is dissolved by alkali lye (paper pulp) is not extracted and separates, send to laundry, choosing is floated operation and is done further processing, after extracting paper pulp, the waste liquid that contains solid content is known as black liquor because of color is black, mainly contains residual alkali in the black liquor, water and the alkali lignin that is dissolved in the alkali lye, hemicellulose and a spot of inorganic salt and other material.
The black liquid treating method of using at present is to concentrate the organic matter of burning in the black liquor, reclaims heat energy and alkali.Main method has flocculation-precipitation method, microorganism treatment, and the processing method of chemical recovery or several technology combinations etc., the waste water quality of handling through these methods can not satisfy discharge standard.The water conductivity that adopts this method to handle drops to 0.23ms/cm, and COD reduces to below the 100mg/L, and water quality is as clear as crystal, and is recyclable, and the rate of recovery reaches about 50%.
The Chinese patent publication number is that CN111671A discloses a kind of black liquid processing and recovery and utilization technology, it is characterized in that under normal temperature, normal pressure, neutrallty condition, with CY series coagulant the cohesion of the suspended matter in black liquid back is filtered, filtrate is discharging after the anaerobic-aerobic biological method is handled; After the filter residue oven dry, send common solid combustion stove to burn and produce steam; Burn the back residue and add Ca (OH) 2 aqueous solution causticizations recovery alkali.The method is used a large amount of CY series coagulants, and complicated operation is unfavorable for industrialized production.
The Chinese patent publication number is that CN101402500A discloses film treatment method for black liquor from papermaking.This invention comprises black liquid after filtration behind the bag filtration, obtain filter residue and filtrate 1, filtrate 1 enters the micro-filtration membrane separator, obtain concentrate 1 and filtrate 2, filtrate 2 enters the NF membrane separator again, acquisition contains the filtrate of alkali and contains the concentrate of lignin and hemicellulose, and filter residue and concentrate be through evaporator evaporation, and contains the sode ash after alkali filtrate is returned recycle or sent to the dissolving boiler combustion.It is relatively poor that the method is filtered the circulating water quality that obtains, and can only be used as first section general flushing water.
Although what said method had comes into operation, but from producing, do not have higher production efficiency, its shortcoming mainly shows: 1. the interpolation of precipitating agent makes bulky grain precipitations such as suspended matter in the black liquor and colloid, and the method for adding precipitating agent can increase the input of resource; 2. preliminary sedimentation tank, medium sediment pool, selecting for use of final deposition pool adopt various settling tanks to come the sedimentation pollutants in waste water, and floor space is big, and under the situation that land used is in short supply, the method should not adopt at present; 3. the employing of biological method selects for use biological method to handle black liquor, and the culturing sludge time is long, not anti-high punching press water, and length consuming time is unfavorable for the Large Scale and Continuous equalization.
Summary of the invention:
The purpose of this invention is to provide a kind of new method and device thereof of handling black liquid acid out waste liquid, can reduce discharge of wastewater, protection environment, conserve water resource.
The present invention is exclusively used in the method for handling black liquid acid out waste liquid, described black liquid acid out waste liquid is that black liquor is by adding acid, separate out remaining waste liquid behind a large amount of price product lignin, wherein the pH value of feed liquid becomes 2-4 by original 11-12, and COD reduces to 30-60g/L by original 110-120.
Above-mentioned black liquid acid out waste liquid after filtering, the 1-5um filter bag is removed wherein large granular impurity and suspended matter; Successively by milipore filter, NF membrane and reverse osmosis membrane, milipore filter is removed macromolecular suspended matter again; NF membrane is removed the salt of most big molecule and part; Reverse osmosis membrane is removed most organic molecule and most salt.Acquisition filters out the clear water of lignin and hemicellulose.And the process of handling is continuous.
Described milipore filter aperture 1nm~20nm, NF membrane aperture 1-2nm, reverse osmosis membrane aperture 0.1nm~1nm.The material of milipore filter, NF membrane and reverse osmosis membrane assembly is an organic polymer, and wherein the face material is cellulose derivative class, polysulfones or polyamide-based, and the face backing material is polyesters or TPO.And described milipore filter, NF membrane, reverse osmosis membrane are a kind of of board-like film, rolled film, tubular membrane and hollow-fibre membrane.
The ultra-filtration process operating temperature is 10-30 ℃, and pressure is 0.05-1.0MPa; The nanofiltration process operating temperature is 10-40 ℃, and pressure is 1.0-2.5MPa; The reverse osmosis process operating temperature is 10-40 ℃, and pressure is 2-4MPa.
Handle the supporting device of black liquid acid out waste liquid method with the present invention, except milipore filter, NF membrane and reverse osmosis membrane, auxiliary equipment comprises high-pressure hydraulic pump, water tank and various Pressure gauge.
The feature of membrane processing method is: the operating condition gentleness, can carry out at normal temperatures; Can use continuously, only need to change membrane module midway, the membrane module of pulling down can be reused after cleaning; Less energy consumption, processing cost is low; The separative efficiency height, the experiment rate of recovery reaches 50%, and the rate of recovery can reach about 70% in the actual production continuously.
Advantage of the present invention is to make part water enter the production upstream, and recycle reduces the discharging of waste water, the conserve water resource.This method can alleviate the load of film, and the film when reducing operation pollutes, and further reduces cost of investment, realizes the reuse of water simultaneously, is suitable for handling black liquid acid out waste liquid.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1:
With 60 liters of COD is 56g/L, the black liquor acid out waste liquid that electricity is led to 1.008ms/cm carries out prefiltration by 1 μ m filter bag, it is 28 ℃ in temperature then, pressure is to be the rolling ultrafiltration membrane system of 20LMH through membrane flux under the condition of 0.5MPa, filter liquor is 28 ℃ in temperature again, pressure is to be the rolling NF membrane system of 6LMH through membrane flux under the condition of 2.25MPa, filter liquor is 28 ℃ in temperature again, pressure is to be the reverse osmosis membrane system of 8LMH through membrane flux under the condition of 2.5MPa, and final concentrate volume is 30 liters, 30 liters of penetrating fluid volumes, COD is 100mg/L, water quality is limpid, and electricity is led and is can satisfy standards for industrial water usage by 0.23ms/cm.
Embodiment 2:
With 60 liters of COD is 56g/L, the black liquor acid out waste liquid that electricity is led to 1.008ms/cm carries out prefiltration by 1 μ m filter bag, it is 30 ℃ in temperature then, pressure is to be the rolling ultrafiltration membrane system of 30LMH through membrane flux under the condition of 1.0MPa, filter liquor is 28 ℃ in temperature again, pressure is to be the rolling NF membrane system of 6LMH through membrane flux under the condition of 2.25MPa, filter liquor is 28 ℃ in temperature again, pressure is to be the reverse osmosis membrane system of 8LMH through membrane flux under the condition of 2.5MPa, and final concentrate volume is 30 liters, 30 liters of penetrating fluid volumes, COD is 105mg/L, water quality is limpid, and electricity is led and is can satisfy standards for industrial water usage by 0.33ms/cm.
Embodiment 3:
With 60 liters of COD is 56g/L, the black liquor acid out waste liquid that electricity is led to 1.008ms/cm carries out prefiltration by 1 μ m filter bag, it is 28 ℃ in temperature then, pressure is to be the rolling ultrafiltration membrane system of 20LMH through membrane flux under the condition of 0.5MPa, filter liquor is 35 ℃ in temperature again, pressure is to be the rolling NF membrane system of 8LMH through membrane flux under the condition of 2.5MPa, filter liquor is 36 ℃ in temperature again, pressure is to be the reverse osmosis membrane system of 10LMH through membrane flux under the condition of 3.5MPa, and final concentrate volume is 30 liters, 30 liters of penetrating fluid volumes, COD is 110mg/L, water quality is limpid, and electricity is led and is can satisfy standards for industrial water usage by 0.40ms/cm.

Claims (10)

1. a black liquid acid out waste liquid membrane processing method is characterized in that, described waste liquid is passed through milipore filter, NF membrane and reverse osmosis membrane successively after the 1-5um filter bag filters, and obtains to filter out the clear water of lignin and hemicellulose.
2. black liquid acid out waste liquid membrane processing method as claimed in claim 1 is characterized in that, described milipore filter aperture 1nm~20nm, NF membrane aperture 1~2nm, reverse osmosis membrane aperture 0.1nm~1nm.
3. black liquid acid out waste liquid membrane processing method as claimed in claim 1 or 2, it is characterized in that, the material of described milipore filter, NF membrane and reverse osmosis membrane assembly is an organic polymer, wherein the face material is cellulose derivative class, polysulfones or polyamide-based, and the face backing material is polyesters or TPO.
4. black liquid acid out waste liquid membrane processing method as claimed in claim 1 or 2 is characterized in that described milipore filter, NF membrane, reverse osmosis membrane are a kind of of board-like film, rolled film, tubular membrane and hollow-fibre membrane.
5. black liquid acid out waste liquid membrane processing method as claimed in claim 1 or 2 is characterized in that the ultra-filtration process operating temperature is 10-30 ℃, and pressure is 0.05-1.0MPa; The nanofiltration process operating temperature is 10-40 ℃, and pressure is 1.0-2.5MPa; The reverse osmosis process operating temperature is 10-40 ℃, and pressure is 2.0-4.0MPa.
6. black liquid acid out waste liquid membrane processing method as claimed in claim 1 is characterized in that, described black liquid acid out waste liquid be black liquor by adding acid, separate out remaining waste liquid behind the lignin, the pH value is 2-4, COD is 30-60g/L.
7. black liquid acid out waste liquid membrane processing method as claimed in claim 1 is characterized in that the process of described processing method is continuous.
8. the used device of the described black liquid acid out of claim 1 waste liquid membrane processing method, it is characterized in that, form, described milipore filter aperture 1nm~20nm by milipore filter, NF membrane and reverse osmosis membrane, NF membrane aperture 1-2nm, reverse osmosis membrane aperture 0.1nm~1nm.
9. device as claimed in claim 8, it is characterized in that, the material of described milipore filter, NF membrane and reverse osmosis membrane assembly is an organic polymer, and wherein the face material is cellulose derivative class, polysulfones or polyamide-based, and the face backing material is polyesters or TPO.
10. install as claimed in claim 8 or 9, it is characterized in that described milipore filter, NF membrane, reverse osmosis membrane are a kind of of board-like film, rolled film, tubular membrane and hollow-fibre membrane.
CN 201010140224 2010-04-07 2010-04-07 Method and device for treating paper-making black liquid acid-precipitation waste liquid film Pending CN101812813A (en)

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CN 201010140224 CN101812813A (en) 2010-04-07 2010-04-07 Method and device for treating paper-making black liquid acid-precipitation waste liquid film

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CN 201010140224 CN101812813A (en) 2010-04-07 2010-04-07 Method and device for treating paper-making black liquid acid-precipitation waste liquid film

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101948192A (en) * 2010-08-31 2011-01-19 长沙绿芯科技有限公司 Membrane technology-based papermaking black liquor high-efficiency comprehensive treatment method
CN102390903A (en) * 2011-09-30 2012-03-28 蒲茂军 Papermaking black liquid membrane treating method
CN103015246A (en) * 2012-12-19 2013-04-03 成都连接流体分离科技有限公司 Method for comprehensively using pulping waste water by sulfite method
CN104053492A (en) * 2011-11-28 2014-09-17 安尼基有限责任公司 Method for reprocessing an aqueous solution containing lignin
CN104674590A (en) * 2013-12-03 2015-06-03 新世膜科技股份有限公司 Treatment method and treatment equipment for papermaking black liquid
CN110804891A (en) * 2019-07-23 2020-02-18 黑龙江如柏科技有限公司 Combined treatment process for papermaking pulp

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1184785A (en) * 1997-12-11 1998-06-17 尤俊洪 Method and equipment for quickly treating waste water for paper mill
CN1193606A (en) * 1998-02-14 1998-09-23 朱树文 Method for recovering and purifying black liquor in papermaking process
CN101285277A (en) * 2008-04-30 2008-10-15 宜宾长毅浆粕有限责任公司 Hyperfiltration process of pulping and digesting black liquor
CN101343122A (en) * 2008-08-19 2009-01-14 贾向东 Regeneration treatment method and device for black liquor of papermaking
CN101402500A (en) * 2008-11-18 2009-04-08 中南大学 Film treatment method for black liquor from papermaking

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1184785A (en) * 1997-12-11 1998-06-17 尤俊洪 Method and equipment for quickly treating waste water for paper mill
CN1193606A (en) * 1998-02-14 1998-09-23 朱树文 Method for recovering and purifying black liquor in papermaking process
CN101285277A (en) * 2008-04-30 2008-10-15 宜宾长毅浆粕有限责任公司 Hyperfiltration process of pulping and digesting black liquor
CN101343122A (en) * 2008-08-19 2009-01-14 贾向东 Regeneration treatment method and device for black liquor of papermaking
CN101402500A (en) * 2008-11-18 2009-04-08 中南大学 Film treatment method for black liquor from papermaking

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Title
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101948192A (en) * 2010-08-31 2011-01-19 长沙绿芯科技有限公司 Membrane technology-based papermaking black liquor high-efficiency comprehensive treatment method
CN102390903A (en) * 2011-09-30 2012-03-28 蒲茂军 Papermaking black liquid membrane treating method
CN104053492A (en) * 2011-11-28 2014-09-17 安尼基有限责任公司 Method for reprocessing an aqueous solution containing lignin
CN103015246A (en) * 2012-12-19 2013-04-03 成都连接流体分离科技有限公司 Method for comprehensively using pulping waste water by sulfite method
CN104674590A (en) * 2013-12-03 2015-06-03 新世膜科技股份有限公司 Treatment method and treatment equipment for papermaking black liquid
CN104674590B (en) * 2013-12-03 2018-01-26 新世膜科技股份有限公司 The processing method and its processing equipment of black liquid
CN110804891A (en) * 2019-07-23 2020-02-18 黑龙江如柏科技有限公司 Combined treatment process for papermaking pulp
CN110804891B (en) * 2019-07-23 2021-08-03 黑龙江如柏科技有限公司 Combined treatment process for papermaking pulp

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Open date: 20100825