CN105525525A - Chemical fiber slurry cellulose alkali squeezing liquid treatment and recovery technology - Google Patents
Chemical fiber slurry cellulose alkali squeezing liquid treatment and recovery technology Download PDFInfo
- Publication number
- CN105525525A CN105525525A CN201410577233.8A CN201410577233A CN105525525A CN 105525525 A CN105525525 A CN 105525525A CN 201410577233 A CN201410577233 A CN 201410577233A CN 105525525 A CN105525525 A CN 105525525A
- Authority
- CN
- China
- Prior art keywords
- hemicellulose
- inorganic material
- material film
- alkali
- pressed liquor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a chemical fiber slurry cellulose alkali squeezing liquid treatment and recovery technology. The technology mainly comprises first-grade film separation, second-grade film separation, hemicellulose precipitation, third-grade film separation and hemicellulose recovery. The invention provides a novel technology for recovering hemicellulose and alkali from an alkali squeezing liquid. Compared with the prior art utilizing a nanofiltration system for recovering alkali, the treatment and recovery technology provided by the invention utilizes an inorganic material membrane to recover alkali, has simple pretreatment processes and has system operation stability, a long cleaning period and a high alkali recovery rate.
Description
Technical field
The present invention relates to three-protection design, particularly relate to the process recovery process of a kind of Pulp Fibers element alkali pressed liquor.
Background technology
In the viscose (artificial silk) being raw material with chemical fiber pulp (plant cellulose such as wood pulp or cotton pulp, straw pulp, bamboo pulp, reed pulp) production in process, cellulose alkali liquor treating process is the first step manufacturing viscose.The manufacture requirements of usual fiber product reaches more than 92% (being not less than 90%) as raw-material chemical cellulose purity.Because its raw material is still containing more hemicellulose, therefore with aqueous slkali, hemicellulose must be dissolved out in impregnation technology, the cellulose of high strength could be obtained.Hemicellulose concentration is high, will produce extremely adverse influence to cellulose viscose manufacturing technique and end product quality.
Alkali pressed liquor is due to containing highly basic, and must carry out special process could not to environmental effects.And due to output huge, cause more serious problem.For reducing production cost, reduce alkaline consumption, protection of the environment, the recycling of alkali must be carried out.The process of alkali pressed liquor is insoluble problem all the time.Such as, in the production process of pulp, hemicellulose inevitably produces together with alkali in expressing process.A certain amount of hemicellulose can being accepted in production process, when going beyond the limit, when viscose acetal fibre is produced and quality has an impact, then must process.Therefore, in recycling alkali lye process, the content of hemicellulose also must be reduced to below certain limit, to guarantee that in alkali reuse process, half fiber can not be accumulated, and can not affect viscose glue production process and product quality.
China once mainly adopted this conventional art of dialysis to reach the object recycling alkali lye.Because traditional dialysis reclaims alkali pressed liquor inefficiency, contaminated environment, and take larger construction area, the membrane separation technique be progressively quickly developed in recent years replaced.Adopt Nanofiltration Membrane Separation Technology and equipment, the hemicellulose in alkali lye and impurity thereof are effectively separated, thus reach the object of the hemicellulose removed in press lye.But the NF membrane adopted in production process at present, due to the restriction of membrane material and film group structure, needs complicated preliminary treatment.Simultaneously in the process being separated hemicellulose, hemicellulose is the highest only can be concentrated to 70-100g/L, and now the rate of recovery of alkali only can reach 50-70%.And in order to system can stable operation, industrially usually do not reach These parameters.If improve alkali recovery, then need to add a large amount of water-dialyzing, the alkali cleaning in hemicellulose concentrate is gone out to permeate end.Although now alkali is purified, the paper mill wastewater obtained, by Macrodilution, can not meet the concentration of lye needed for impregnation technology, cannot direct reuse in technique, have to pass through concentrated, until dipping desired concn could reuse.Simultaneously due in original technique, the restriction of membrane material and membrane component structure, processing procedure poor stability, needs to carry out perfect preliminary treatment.
Summary of the invention
Object of the present invention, exactly in order to solve above-mentioned prior art Problems existing, provides the process recovery process of a kind of Pulp Fibers element alkali pressed liquor.
In order to achieve the above object, present invention employs following technical scheme: a kind of process recovery process of Pulp Fibers element alkali pressed liquor, alkali pressed liquor is sent into one-level inorganic material film separation system, hemicellulose is trapped and forms hemicellulose concentrate, part alkali lye is purified through film, can direct reuse.
One-level inorganic material film separation system gained hemicellulose concentrate is sent into secondary inorganic material film separation system, add water dialysis, and hemicellulose is trapped and forms hemicellulose concentrate, and permeate is alkali lye, can direct reuse.
The molecular weight that dams of the inorganic material film that described one-level inorganic material film separation system and secondary inorganic material film separation system adopt is 100-5000, or the aperture of film is 1-10 nanometer.
The operating temperature that described one-level inorganic material film separation system and secondary inorganic material film separation system adopt controls at 50-60 DEG C, and operating pressure controls at 0.1-3Mpa.
The inorganic material of described inorganic material film is selected from one or more in alundum (Al2O3), zirconium dioxide, titanium dioxide, stainless steel, alloy, nickel alloy or carborundum.
Described inorganic material film adopts tubular type or board-like film.
Described inorganic material film adopts tubular membrane, and adopt cross-flow filtration, film surface velocity controls at 0.5-5 meter per second.
Described inorganic material film adopts tubular membrane, and operating pressure controls at 0.1-3Mpa.
By secondary inorganic material film separation system gained hemicellulose concentrate acid adding, hemicellulose is separated out, obtain the turbid liquid of solid phase hemicellulose, turbid liquid is sent into three grades of film separation systems, hemicellulose is trapped, add water-dialyzing and wash the hemicellulose be trapped, the hemicellulose slurry be purified.
The membrane aperture that three grades of described film separation systems adopt is 1-100nm, and the film adopted is polymer material film or inorganic material film; Described macromolecular material is selected from the mixture of one or more in polyether sulfone, polysulfones, armaticity polysulfones, Kynoar, polyvinyl chloride, polyketone, polyether-ketone, polytetrafluoroethylene (PTFE), polyethylene or polyamide; Described inorganic material is selected from the one in alundum (Al2O3), zirconium dioxide, titanium dioxide, stainless steel, alloy, nickel alloy or carborundum.
The invention provides the technique reclaiming hemicellulose and alkali in a kind of chemically slurry alkali pressed liquor newly.Adopt nanofiltration system to reclaim compared with alkali technique with existing technique, in the present invention, adopt inoranic membrane directly to process alkali pressed liquor, simplify pretreating process.Owing to adopting inoranic membrane, film is anti-pollution more, and the life-span is longer.System is more stable.Operating cost is lower.The present invention achieves the recovery of hemicellulose in pressed liquor simultaneously, and the hemicellulose of acquisition can be used as xylose production raw material.
The process recovery process of Pulp Fibers element alkali pressed liquor of the present invention has following significant advantage and disadvantage:
1, pretreating process is simplified;
2, system is more stable, and film operation maintenance is simpler;
3, the longer service life of film;
4, the paper mill wastewater reclaimed remains unchanged, without the need to through concentrated, and can direct reuse;
5, the recovery of hemicellulose is realized, and can the recycling of high added value.
Detailed description of the invention
In alkali pressed liquor in the present invention, paper mill wastewater is 150-300g/L, and hemicellulose level is 10-60g/L.
The raw material sources of dipping can be timber, cotton, straw, sugarcane, bamboo, reed, stem, leaf fiber or said mixture containing fiber.Preferred wood pulp pulp is as cellulose origin.Wood pulp source comprises cork, hardwood.In cellulose, the content of half fibre can reach 30%.
Maceration extract after alkali treatment, after plate compression, obtains press lye.Its naoh concentration is usually between 150-300g/L, and half fine content is different according to raw material difference, usually between 10-60g/L.Through being pumped into one-level film separation system.The molecular weight that dams of one-level film is 100-5000, or the aperture of film is 1-10 nanometer.Operating pressure 0.3-2MPa, 50-60 DEG C of operation, NaOH and water are through film, and hemicellulose tunicle retains concentrated.Usual hemicellulose is concentrated to 50-100g/L, and the content 1-10g/L of hemicellulose in permeate, alkali concn is identical with feeding liquid.Permeate is inserted in storage tank for subsequent use, can be directly used in impregnation technology.Now secondary membrane piece-rate system continuation process sent into by the concentrate of one-level film separation system.One-level film separation system alkali recovery is usually at 50-85%.
Through the hemicellulose concentrate of one-level film separation system initial concentration, through being pumped into secondary membrane piece-rate system.The molecular weight that dams of one-level film is the aperture of 100-5000 or film is 1-10 nanometer.Operating pressure 0.25-2MPa, 50-60 DEG C of operation, add water dialysis, and NaOH and water are through film, and hemicellulose tunicle retains concentrated.Through the process of secondary membrane piece-rate system, alkali recovery improves further.
Through one-level film separation system and the process of secondary membrane piece-rate system, alkali recovery is the highest can reach 95%.
The hemicellulose concentrate concentrated through secondary membrane piece-rate system enters three grades of film separation systems.
The recovery of hemicellulose can adopt following in and technique, the concentrate by secondary membrane piece-rate system is placed in tank, slowly adds inorganic acid, as sulfuric acid, nitric acid, hydrochloric acid, citric acid, phosphoric acid etc.Along with the progressively reduction of pH value, hemicellulose is separated out.Obtain the turbid liquid of hemicellulose.This turbid liquid enters three grades of film separation systems.The aperture of damming of three grades of films is 1-100nm.Operating pressure 0.1-4MPa, temperature 10-80 DEG C of operation, preferred 0.25-0.7MPa, 30-60 DEG C of operation, salt and water are through film, and hemicellulose tunicle retains concentrated.Add a certain amount of water-dialyzing concentrated solution for washing, make the salt of concentrate end through film, hemicellulose is purified further.Dialysis limit, limit concentrates.Dialysis terminates, and it is dry that suspension sends into spray drying tower spray, obtains hemicellulose powder.
Obtain hemicellulose turbid liquid in above-mentioned technique, also can pass through centrifugation, hemicellulose precipitates, then drying obtains sterling.Or by filtering, be separated and obtain hemicellulose solid, drying obtains sterling.
Present invention also offers a kind of alkali recovery process of improvement, specifically, alkali pressed liquor enters one-level film separation system, and the concentrate of one-level film separation system enters secondary membrane piece-rate system, and the filter liquor of secondary membrane piece-rate system is partly or entirely again through the process of one-level film separation system.The filtrate of one-level film separation system and the filtrate direct reuse of part secondary membrane piece-rate system are to impregnation technology.The filter liquor of this technique to secondary membrane piece-rate system purifies again, remove further in secondary membrane piece-rate system filter liquor through hemicellulose, improve the purity of secondary membrane piece-rate system filter liquor alkali lye further.This technique is for the impregnation technology viscose production technology higher to NaOH purity requirement.
Embodiment 1
Alkali pressed liquor 100 cubic metres, in charging, naoh concentration is 250g/L, and hemicellulose level is 25g/L.Enter one-level film separation system temperature 50 degrees Celsius, the aperture of damming of film is 5nm.Operate under pressure 2MPa.When being concentrated to hemicellulose cellulose content 80g/L, entering secondary membrane system and to add water dialysis.The aperture of damming of secondary membrane is 5nm.One-level film separation system, secondary membrane piece-rate system membrane filtration fluid are placed in that to leach flow container for subsequent use.Total filter liquor hemicellulose level 7g/L.Be back to impregnation technology.
Embodiment 2
Chemical recovery system film concentrate 5 cubic metres, wherein hemicellulose level 300g/L, naoh concentration 60g/L.To add with NaOH equimolar 30% sulfuric acid solution in the container placing above-mentioned concentrate, limit edged stirs.Hemicellulose is separated out.Leave standstill more than 2 hours.Entering aperture of damming is that three grades of film separation systems of 50nm are separated.At 0.6MPa pressure, keep film surface velocity 5 meter per second.First be concentrated to 2-3 cubic meter volume, then the dialysis that adds water, amount of water 10-15 cubic meter.Obtain the hemicellulose concentrate that can directly reclaim.
Embodiment 3
Alkali pressed liquor 100 cubic metres, in charging, naoh concentration is 200g/L, and hemicellulose level is 20g/L.Enter one-level film separation system temperature 50 degrees Celsius, operate under pressure 0.4MPa.When being concentrated to hemicellulose level 82g/L, entering secondary membrane system and to add water dialysis.One-level film separation system, secondary membrane piece-rate system membrane filtration fluid are placed in that to leach flow container for subsequent use.
Claims (10)
1. a process recovery process for Pulp Fibers element alkali pressed liquor, is characterized in that, alkali pressed liquor is sent into one-level inorganic material film separation system, and hemicellulose is trapped and forms hemicellulose concentrate, and a part of alkali lye is purified through film, can direct reuse.
2. the process recovery process of cellulose alkali pressed liquor according to claim 1, it is characterized in that, one-level inorganic material film separation system gained hemicellulose concentrate is sent into secondary inorganic material film separation system, add water dialysis, hemicellulose is trapped and forms hemicellulose concentrate, permeate is alkali lye, can direct reuse.
3. the process recovery process of cellulose alkali pressed liquor according to claim 2, it is characterized in that: the molecular weight that dams of the inorganic material film that described one-level inorganic material film separation system and secondary inorganic material film separation system adopt is 100-5000, or the aperture of film is 1-10 nanometer.
4. the process recovery process of cellulose alkali pressed liquor according to claim 2, it is characterized in that: the operating temperature that described one-level inorganic material film separation system and secondary inorganic material film separation system adopt controls at 50-60 DEG C, and operating pressure controls at 0.1-3Mpa.
5. the process recovery process of cellulose alkali pressed liquor according to claim 3, is characterized in that: the inorganic material of described inorganic material film is selected from one or more in alundum (Al2O3), zirconium dioxide, titanium dioxide, stainless steel, alloy, nickel alloy or carborundum.
6. the process recovery process of cellulose alkali pressed liquor according to claim 3, is characterized in that: described inorganic material film adopts tubular type or board-like film.
7. the treatment process of cellulose alkali pressed liquor according to claim 3, is characterized in that: described inorganic material film adopts tubular membrane, and adopt cross-flow filtration, film surface velocity controls at 0.5-5 meter per second.
8. the treatment process of cellulose alkali pressed liquor according to claim 3, is characterized in that: described inorganic material film adopts tubular membrane, and operating pressure controls at 0.1-3Mpa.
9. the treatment process of cellulose alkali pressed liquor according to claim 2, it is characterized in that: by secondary inorganic material film separation system gained hemicellulose concentrate acid adding, hemicellulose is separated out, obtain the turbid liquid of solid phase hemicellulose, turbid liquid is sent into three grades of film separation systems, hemicellulose is trapped, and adds water-dialyzing and washs the hemicellulose be trapped, the hemicellulose slurry be purified.
10. the treatment process of cellulose alkali pressed liquor according to claim 9, is characterized in that: the membrane aperture that three grades of described film separation systems adopt is 1-100nm, and the film adopted is polymer material film or inorganic material film; Described macromolecular material is selected from the mixture of one or more in polyether sulfone, polysulfones, armaticity polysulfones, Kynoar, polyvinyl chloride, polyketone, polyether-ketone, polytetrafluoroethylene (PTFE), polyethylene or polyamide; Described inorganic material is selected from the one in alundum (Al2O3), zirconium dioxide, titanium dioxide, stainless steel, alloy, nickel alloy or carborundum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410577233.8A CN105525525A (en) | 2014-10-24 | 2014-10-24 | Chemical fiber slurry cellulose alkali squeezing liquid treatment and recovery technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410577233.8A CN105525525A (en) | 2014-10-24 | 2014-10-24 | Chemical fiber slurry cellulose alkali squeezing liquid treatment and recovery technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105525525A true CN105525525A (en) | 2016-04-27 |
Family
ID=55768022
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410577233.8A Pending CN105525525A (en) | 2014-10-24 | 2014-10-24 | Chemical fiber slurry cellulose alkali squeezing liquid treatment and recovery technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105525525A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243248A (en) * | 2016-08-23 | 2016-12-21 | 南京工业大学 | Method for extracting hemicellulose from recovered alkali in viscose fiber production |
| CN108715765A (en) * | 2018-06-19 | 2018-10-30 | 南京工业大学 | Method for preparing hemicellulose-based water-retaining agent by using hemicellulose emulsion through microchannel reaction device |
| CN109021146A (en) * | 2018-08-01 | 2018-12-18 | 辽宁莱特莱德环境工程有限公司 | For squeezing the method and device thereof of spent lye recycling in production process of viscose fiber |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3935022A (en) * | 1973-07-23 | 1976-01-27 | Hannes Sihtola | Method for the removal of hemicellulose from hemicellulose-containing caustic liquors |
| 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 |
| CN102943322A (en) * | 2012-11-09 | 2013-02-27 | 大连山元机械制造有限公司 | Treatment device and recovering method for pressing alkali |
| 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 |
| CN103864961A (en) * | 2014-03-13 | 2014-06-18 | 唐山三友集团兴达化纤有限公司 | Method for extracting semi-fibers of regenerated cellulose fiber impregnation liquid and application of semi-fibers |
-
2014
- 2014-10-24 CN CN201410577233.8A patent/CN105525525A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3935022A (en) * | 1973-07-23 | 1976-01-27 | Hannes Sihtola | Method for the removal of hemicellulose from hemicellulose-containing caustic liquors |
| 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 |
| CN102943322A (en) * | 2012-11-09 | 2013-02-27 | 大连山元机械制造有限公司 | Treatment device and recovering method for pressing alkali |
| 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 |
| CN103864961A (en) * | 2014-03-13 | 2014-06-18 | 唐山三友集团兴达化纤有限公司 | Method for extracting semi-fibers of regenerated cellulose fiber impregnation liquid and application of semi-fibers |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243248A (en) * | 2016-08-23 | 2016-12-21 | 南京工业大学 | Method for extracting hemicellulose from recovered alkali in viscose fiber production |
| CN108715765A (en) * | 2018-06-19 | 2018-10-30 | 南京工业大学 | Method for preparing hemicellulose-based water-retaining agent by using hemicellulose emulsion through microchannel reaction device |
| CN108715765B (en) * | 2018-06-19 | 2020-09-08 | 南京工业大学 | Method for preparing hemicellulose-based water-retaining agent by using hemicellulose emulsion through microchannel reaction device |
| CN109021146A (en) * | 2018-08-01 | 2018-12-18 | 辽宁莱特莱德环境工程有限公司 | For squeezing the method and device thereof of spent lye recycling in production process of viscose fiber |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103572635B (en) | The process recovery process of chemical fiber pulp cellulose alkali pressed liquor | |
| CN106242101B (en) | The processing recovery process of alkali pressed liquor in production process of viscose fiber | |
| CN1197784C (en) | Method for recovering alkali and hemicellulose from chemical fibre waste liquid | |
| CN101284913A (en) | Preparation method of cellulose membrane by using ion liquid as solvent | |
| CN101274947B (en) | Method for extracting lignosulphonate from sodium sulfite bamboo pulp waste liquor | |
| CN107433143B (en) | Polyelectrolyte-loaded antibacterial cellulose nanofiltration membrane and preparation method thereof | |
| CN103397407B (en) | The ultrafiltration pretreatment technique of pressed liquor electrodialysis alkali collection in viscose production | |
| CN105525525A (en) | Chemical fiber slurry cellulose alkali squeezing liquid treatment and recovery technology | |
| CN102167465A (en) | Recovery method of spinning waste liquor by means of concentrating | |
| CN105525389A (en) | Chemical pulp cellulose alkali squeezing liquid zero-discharge recovery technology | |
| CN106237859B (en) | The alkali recovery process of alkali pressed liquor in production process of viscose fiber | |
| CN103864961A (en) | Method for extracting semi-fibers of regenerated cellulose fiber impregnation liquid and application of semi-fibers | |
| CN101392417A (en) | Method for recovering ion liquid solvent from cellulose spinning by combination method | |
| CN104328452B (en) | Production process of gluconic acid by bipolar membrane electrodialysis method | |
| CN104311702A (en) | Method for extracting hemicellulose from viscose squeezing alkali liquor | |
| CN103669069B (en) | Spentsulfiteliquor process recovery process | |
| CN103397405B (en) | Pretreatment technique for recovering pressed liquor electrodialysis alkali in viscose fiber production | |
| CN104652156B (en) | Method for preparation of lignosulfonate and cogeneration of microcrystalline cellulose from corn cob residues | |
| Liu et al. | Purification of hemicelluloses in pre-hydrolysis liquor of kraft-based dissolving pulp production process using activated carbon and ion-exchange resin adsorption followed by nanofiltration | |
| CN106468032A (en) | The method and device of lignin is extracted a kind of black liquor from sulfate pulping | |
| CN107032533A (en) | A kind of integrated membrane process method for desalting seawater | |
| CN106676931B (en) | A kind of fully separating method of black liquid component | |
| EP2753584A1 (en) | Plant and procedure for recovering used brine from dyeing vats | |
| CN104311706A (en) | Electrodialysis technology for exacting semi fibers by using viscose fiber pressed alkali liquor as raw materials | |
| CN111661967A (en) | System and method for recovering alkali in viscose fiber production squeezing waste liquid by using double-membrane method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| CB02 | Change of applicant information |
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 |
|
| COR | Change of bibliographic data | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
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. |
|
| CB02 | Change of applicant information | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160427 |
|
| RJ01 | Rejection of invention patent application after publication |