CN103147334B - Waste paper deinking method using mixed enzyme - Google Patents
Waste paper deinking method using mixed enzyme Download PDFInfo
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- CN103147334B CN103147334B CN201210574470.XA CN201210574470A CN103147334B CN 103147334 B CN103147334 B CN 103147334B CN 201210574470 A CN201210574470 A CN 201210574470A CN 103147334 B CN103147334 B CN 103147334B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/64—Paper recycling
Abstract
The invention relates to a waste paper deinking method using mixed enzyme. The waste paper deinking method using the mixed enzyme mainly solves the problem in the prior art of poor deinking effect. The waste paper deinking method using the mixed enzyme includes a first step of obtaining serous fluid A by stirring and mixing deinking agent aqueous solution with waste papers under the condition that potential of hydrogen (pH) is equal to 7.0 to 7.5, wherein the deinking agent aqueous solution comprises sodium aliphatate which is a source of vegetable oil and/ or non-ionic surface active agent which is expressed by sylvite, formula RO(CH2CH2O)nH, wherein R is C10 to C18 of alkyl group, and n is equal to 3 to 12, and the deinking agent aqueous solution further comprises cellulase, lipase and amylase, a second step of adding water to the serous fluid A and obtaining serous fluid B by mediating the pH to be equal to 6.5 to 6.9, and a third step of obtaining deinking serous fluid by conducting flotation process on the serous fluid B. The waste paper deinking method using the mixed enzyme has the advantages of being capable of well solving the technical problems and being used in waste paper deinking production.
Description
Technical field
The present invention relates to adopt the deinking process for waste paper of mixed enzyme.
Background technology
Waste paper regenerated utilization meets the growth requirement of low-carbon (LC) conservation-minded society.Manufacture high-quality paper product for the fiber that makes to reclaim meets from waste paper, conventionally the ink in waste paper need to be removed.
The method of tradition deinking is chemical method.In chemical method deinking process for waste paper, conventionally can use NaOH, sodium metasilicate, chelating agent, hydrogen peroxide, dispersant, trapping agent and agglomerant.In order to make ink particle fully depart from the surface of waste paper fibre, Chemical Deinking technique need to be carried out conventionally in the medium of higher alkalisation, and for example pH is even up to 11.Due to the use of high alkalinity medium in Chemical Deinking technique, cause the flavescence of cellulose fiber peacekeeping ligno-ccllulose, in order to obtain the recycled writing paper fiber of high whiteness, in deinking process, also need to use oxidative bleaches (for example hydrogen peroxide) or reducibility bleaching agent (for example industrial insurance powder) for this reason.The existence of high alkalinity medium in deinking process, it is reported and also can cause paper pulp fiber recurring structure to change, and makes the degradations such as the paper strength that makes, simultaneously because a large amount of employings of chemicals all cause adverse influence to production equipment and environment.
In view of the foregoing, occurred the method for Researches of Enzymatic-Deinking on Waste Paper, Enzymatic Deinking is owing to can reducing the use amount of chemicals thereby environmental protection more.
Sui Zhenying etc. (mixed enzyme is for the research [J] of laser printing deinking. Chemical Engineering, 2009,37 (9): 44～47) studied cellulase, amylase and lipase and their mixed enzyme, mixed enzyme and their mixed enzyme in different proportionings, temperature, the impact of pH value on deinking efficiency.
Chinese patent literature CN101718050A (applying date 2009.11.13, an open day 2010.06.02) a kind of method of Researches of Enzymatic-Deinking on Waste Paper disclosed, in its deinking agent adopting, comprise cellulase, lipase, amylase, zytase, surfactant, comprise following technological process: the preparation of (1) deinking agent: one or more make complex enzyme in cellulase, to add alkaline lipase, amylase, zytase; In complex enzyme, each component ratio is: 2000～10000u cellulase, 10000～100000u alkaline lipase, 1000～5000u zytase and 8000～15000u amylase, then in described complex enzyme, add the surfactant of 0.05～0.15 kilogram to obtain described deinking agent; (2) pulper pulping: add the water of 40～60 DEG C in pulper, carry out shredded paper operation after dropping into deinking agent and sodium metasilicate in waste paper; (3) enter FLOTATION SEPARATION ink operation and obtain deinking slurries.From above-mentioned disclosed content, can find out, the method still needs to use alkaline matter sodium metasilicate.Entirely so it does not record about pH actual conditions in claimed technical scheme, but owing to having used sodium metasilicate, and the deinking wastewater pH listing in the table of the 4/5th page, its description 8.08 can find out, the pH in its deinking process should be more than 8.
(its priority data is 10164835.0 2010.06.03EP and 61/303 to another part patent documentation CN102753753A, 828 2010.02.12US) a kind of Researches of Enzymatic-Deinking on Waste Paper method is also disclosed subsequently, as follows to its claimed technical scheme summary: (a) under the denseness at least about 3%, the printing paper slurrying that wherein at least 25wt% is old newsprint to be obtained to slush pulp; (b) process described slush pulp by deinking system, described system comprises: (i) lipase and at least one are selected from the combination of the second enzyme of amylase, xylosidase or cellulase, and (ii) non-ionic surface active agent of its amount for effectively ink being discharged from described slush pulp; (c) in deinking step, separate the ink discharging from described slush pulp, so that the slush pulp of deinking to be provided.It is in deinking, also to comprise alkaline reagent and the soap derived from vegetable oil that the document further discloses its preferred technical scheme in its claim 31.
But there is the poor problem of deinking efficiency in existing mixed enzyme Deinking Technology.
Summary of the invention
There is the poor problem of deinking efficiency in the existing mixed enzyme Deinking Technology that the present invention will solve, a kind of deinking process for waste paper that adopts mixed enzyme is provided, and the method has advantages of that deinking efficiency is good.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: adopt the deinking process for waste paper of mixed enzyme, comprise the steps:
(1) under temperature is 25～55 DEG C, the condition of pH=7.0～7.5, the deinking agent aqueous solution and waste paper are uniformly mixed, and incorporation time is 5～40 minutes, obtains spent pulp liquors A; Wherein the weight ratio that feeds intake of waste paper and the deinking agent aqueous solution is 100: (300～900); The described deinking agent aqueous solution contains anion surfactant and non-ionic surface active agent, in weight ratio, and waste paper: anion surfactant: non-ionic surface active agent is 100: (0.05～0.15): (0.05～1.0); Described anion surfactant is at least one in aliphatic acid potassium or the sodium soap in vegetable oil source; Described non-ionic surface active agent general molecular formula is RO (CH
2cH
2o)
nh, wherein R is C
10～C
18alkyl, n=3～12; In the described deinking agent aqueous solution, go back cellulase 0.2～0.5u/g, lipase 0.3～1.0u/g and amylase 0.2～1.0u/g;
(2), to thin up in spent pulp liquors A and add acidic ph modifier, obtain taking waste paper weight concentration as 0.6～1.0wt%, the spent pulp liquors B of pH=6.5～6.9;
(3) spent pulp liquors B is carried out to flotation processing and obtain deinking slurries.
The temperature of step in technique scheme (1) is preferably 40～50 DEG C.The pH of step (1) is preferably 7.2～7.4.Preferably at least one in soybean oil, sunflower oil, corn oil, rapeseed oil, peanut oil, cottonseed oil, olive oil, tea oil, palm oil or coconut oil of the described vegetable oil of step (1); Further preferred at least one in soybean oil, sunflower oil, corn oil, rapeseed oil, peanut oil, cottonseed oil, olive oil, tea oil; Further preferred at least one in soybean oil, sunflower oil, corn oil, rapeseed oil, peanut oil, cottonseed oil; Most preferably at least one in soybean oil, sunflower oil, corn oil; The anion surfactant that the described anion surfactant of step (1) is the most preferably originated by soybean oil and the anion surfactant of being originated by cottonseed oil form.
The incorporation time of step in technique scheme (1) is preferably 10～20 minutes.R is preferably C
12～C
14alkyl, preferably n=5～10.Described in step (2), pH adjusting agent can be organic acid or inorganic acid, can be also that the aqueous solution is acid salt, but is preferably at least one in EDTA Dipotassium salt or disodium EDTA, ethylenediamine tetra-acetic acid di-ammonium salts.The described pH of step (2) is preferably 6.5～6.8.
The temperature of step in technique scheme (3) flotation is preferably 20～85 DEG C; More preferably 20～60 DEG C of flotation temperatures.Flotation time is 10～30min preferably, more preferably 10～20min.
Technique scheme is applicable to the deinking of various waste paper, and described waste paper can be for example at least one in crushed news, useless laser printing word, useless magazine paper.
For meeting the requirements at the higher level to pulp brightness, technical scheme of the present invention can also increase hydrogen peroxide bleaching operation afterwards in completing steps (1), for example hydrogen peroxide bleaching can: (a) carry out afterwards and between step (2) in step (1); (b) carry out afterwards in step (3).
The connotation that the aliphatic acid potassium of originating as the vegetable oil of anion surfactant in the present invention or sodium soap have is: these aliphatic acid potassium or sodium soap can (i) obtain from vegetable oil saponification, can be also that (ii) soap stock from corresponding vegetable oil industry obtains for originating.The anion surfactant that these two kinds of approach obtain is all applicable to the present invention and has identical result of use, but more to one's profit economically from obtaining with the soap stock of corresponding vegetable oil.
The amount that contains various enzymes in the solution of deinking agent described in the present invention is taking u/g as unit representation, in the time relating to cellulase content, its implication is specified by light industry standard QB 2583-2003, in the time relating to lipase, specified by GB/T 23535-2009, while relating to amylase, specified by GB 8275-2009.As long as the enzyme dosage representing with u/g is as described in technique scheme, the source of concrete enzyme used is not particularly limited, and above-mentioned enzyme can use with the form of the zymotic fluid of bacterium producing multi enzyme preparation, can be also the commercially available enzyme product through purifying.In the embodiment of the present invention, all adopt commercially available cellulase (cellulase EC3.2.1.4), commercially available lipase (Lipase EC3,1,1,3), commercially available amylase (α-amylase EC3.2.1.1) is for experiment.
In an embodiment the factor of key point of the present invention is not fixed, so that obtain having more the experimental result of comparativity, not the inventive method only adopts these rigid conditions just can reach object of the present invention, on technical scheme disclosed by the invention basis, those skilled in the art can rationally determine these factors in conjunction with this area customary means.Corresponding to step of the present invention (1), fix following factor at embodiment: in the FORMAX450H high-concentration pulper that step (1) is 12L at cylinder body volume, carry out, the fragment that waste paper is cut into 25mm × 25mm with paper knife is for experiment, and pulper rotating speed is 1500r/min.Corresponding to having fixed following factor in step of the present invention (3) embodiment: step (3) is carried out in the FORMAX of 28L L-100 type flotation cell, taking air as flotation gas, volume of air is taking status of criterion lower volume air intake as 20m
3/ h.
Water, the step (2) in the deinking agent aqueous solution of step in the embodiment of the inventive method (1), used are diluted added water, all adopt running water.Due to the pH fluctuation between 6.5～8.5 conventionally of running water, after can causing the deinking agent aqueous solution to mix with waste paper, exceed the required pH condition of step (1), at this moment for the accurate control of performing step (1) pH, those skilled in the art will know that by under accurate pH test paper or the instruction of accurate pH meter, for example, by adding acidic materials (acetic acid in the mixture to the deinking agent aqueous solution and waste paper formation, hydrochloric acid, sulfuric acid) or add alkali (for example ammoniacal liquor, sodium carbonate, potassium hydroxide, NaOH) pH is controlled to the required value of step (1), and weak acid (for example acetic acid), weak base (for example ammoniacal liquor, sodium carbonate) easier for pH value fine setting operation.
Deinking Efficiency in embodiment, is to adopt Technidyne Color Touch ERIC950 type residual ink analyzer, and the ERIC value of measuring contrast slurries according to international standard ISO-22754-2008 regulated procedure (is expressed as ERIC
contrast slurries) and the ERIC value of the deinking slurries that obtain of step (3) (be expressed as ERIC
deinking slurries), the computing formula of Deinking Efficiency is: Deinking Efficiency=[(ERIC
contrast slurries-ERIC
deinking slurries)/ERIC
contrast slurries] × 100%; Wherein, for measuring Deinking Efficiency, the preparation method of contrast slurries is except the water consumption substitution deinking agent aqueous solution, and all the other operations and condition are all identical with step (1).
Adopt after technical scheme of the present invention, can find out from embodiment, Deinking Efficiency can reach 86.7%, has obtained good technique effect, can be used in the deinking production of waste paper.
Below in conjunction with detailed description of the invention, the present invention will be further described.
Detailed description of the invention
[embodiment 1]
Step (1): under temperature is 45 DEG C, pH=7.3 condition, the deinking agent aqueous solution and waste paper are uniformly mixed in FORMAX450H high-concentration pulper, incorporation time is 15min, obtains spent pulp liquors A; Wherein the weight ratio that feeds intake of waste paper and the deinking agent aqueous solution is 100: 600; The deinking agent aqueous solution contains anion surfactant and non-ionic surface active agent, in weight ratio, and waste paper: anion surfactant: non-ionic surface active agent is 100: 0.10: 0.5; Anion surfactant is the sodium soap in soybean oil source; Non-ionic surface active agent is lauryl alcohol polyoxyethylene (7) ether, i.e. RO (CH in general molecular formula
2cH
2o)
nthe R of H is C
12alkyl, n=7; Cellulase 0.4u/g, lipase 0.6u/g and amylase 0.6u/g in the deinking agent aqueous solution.The deinking agent aqueous solution and waste paper gross weight are 8000 grams.Waste paper is the People's Daily in November, 2011.
Step (2): to thin up in spent pulp liquors A and add acidic ph modifier, obtain taking waste paper weight concentration as 0.8wt%, the spent pulp liquors B of pH=6.7, acidic ph modifier is EDTA2Na.
Step (3): 25 kilograms of waste liquid slurries B are placed in to the flotation of BFORMAX L-100 type flotation cell and obtain deinking slurries.Flotation gas is air, and volume of air is taking status of criterion lower volume air intake as 20m
3/ h.30 DEG C of flotation temperatures, flotation time 15min.
After tested, Deinking Efficiency is 83.4%.For ease of relatively main technological parameter and test result being listed in to table 1 and table 2
[embodiment 2]～[embodiment 20]
Step (1): except anion surfactant changes, other operate all steps (1) with embodiment 1.
Step (2): operate all identical with the step (2) of embodiment 1.
Step (3): except flotation temperature changes, all the other operations are all identical with embodiment 1 step (3).Measure Deinking Efficiency.For ease of relatively the technological parameter of variation and measurement result being listed in to table 1 and table 2.
[embodiment 21]～[embodiment 32]
Step (1): except the weight ratio that feeds intake of temperature, pH, incorporation time, waste paper and the deinking agent aqueous solution, in the waste paper of weight ratio: anion surfactant: the consumption of three kinds of enzymes changes in the R in non-ionic surface active agent, the agent of anion surface active energy, non-ionic surface active agent structure and n, the deinking agent aqueous solution, other operations are all with the step (1) of embodiment 1.
Step (2): except the pH of the concentration of pH adjusting agent, spent pulp liquors B, spent pulp liquors changes, all the other operations are all identical with the step (2) of embodiment 1.
Step (3): except flotation temperature and flotation time change, all the other operations are all identical with embodiment 1 step (3).Measure Deinking Efficiency.For ease of relatively the technological parameter of variation and measurement result being listed in to table 3 and table 4.
[embodiment 33]
Except the waste paper of step (1) adopts useless laser stamping paper, take laser stamping paper through the laser printing of one side black and white, all the other operations are all identical with embodiment 1.After measured, Deinking Efficiency is 83.6%.For ease of relatively, technological parameter and measurement result are listed in to table 3 and table 4.
[embodiment 34]
Adopt useless magazine except step (2) adopts waste paper, all the other operating conditions are all identical with embodiment 1.Wherein useless magazine is " China youth " (periodical publisher of China youth edits and publishes, the 18th phase in 2009) of removing after front cover.After measured, Deinking Efficiency is 82.1%.For ease of relatively, technological parameter and measurement result are listed in to table 3 and table 4.
[comparative example 1]～[comparative example 3]
Except step (1) pH, step (2) pH, step (2) pH adjusting agent change, all the other operating conditions are all identical with embodiment 1.Measure Deinking Efficiency.For ease of relatively, technological parameter and measurement result are listed in to table 3 and table 4.
Finally, as summary of the present invention, the present inventor finds through a large amount of experiments:
One, about vegetable oil source and flotation temperature relation
Flotation temperature between 20～40 DEG C time deinking efficiency by good to poor be sequentially soybean oil ≈ sunflower oil ≈ corn oil > rapeseed oil ≈ peanut oil ≈ cottonseed oil > olive oil ≈ tea oil > palm oil ≈ coconut oil; This also can be confirmed from the data of embodiment 1～embodiment 10.
In the time that flotation temperature is brought up to 45～50 DEG C, in the time that aliphatic acid potassium or sodium are derived from rapeseed oil, peanut oil or cottonseed oil, Deinking Efficiency improves obviously, approach the level in soybean oil, sunflower oil or corn oil source, the deinking efficiency that is derived from soybean oil, sunflower oil, corn oil, olive oil, tea oil increases, and the Deinking Efficiency that is derived from palm oil or coconut oil does not have significant change.This also can be confirmed by the data of embodiment 1～embodiment 20.In the time that flotation temperature is further brought up to 55～60 DEG C, olive oil, tea oil, palm oil, the aliphatic acid potassium in coconut origin source or the deinking efficiency of sodium salt are just fully demonstrated, thereby the fat acid potassium in above-mentioned various fat oils source or the Deinking Efficiency of sodium salt are tending towards close, and these data from embodiment 21～embodiment 23 are confirmed.Therefore, in order to reach good deinking efficiency, soybean oil, sunflower oil, aliphatic acid sylvite or the sodium salt in corn oil source have the widest flotation temperature scope (more preferably selecting 20～60 DEG C), and there is larger temperature range to approach environment temperature, therefore being not only conducive to improve operating flexibility that flotation produces also helps and realizes floatation process and realize energy-saving and cost-reducing, from this angle, next is rapeseed oil, peanut oil, aliphatic acid sylvite or the sodium salt in cottonseed oil source, its preferred flotation temperature scope is 45～60 DEG C, secondly be olive oil again, tea oil, palm oil, coconut oil, its preferred flotation temperature scope is 55～60 DEG C.
Two, about the acidic ph modifier of step (2)
While adopting disodium ethylene diamine tetraacetate, EDTAP dipotassium ethylene diamine tetraacetate, ethylenediamine tetra-acetic acid two ammonium, Deinking Efficiency is suitable, but be all better than other common acid, for example hydrochloric acid, sulfuric acid, phosphoric acid, acetic acid, this can be confirmed from the data of embodiment 1, embodiment 24～embodiment 26.
Three, the aliphatic acid sylvite (or sodium) in soybean oil source uses with the aliphatic acid sylvite (or sodium salt) in cottonseed oil source simultaneously
For unaccountable reason, both have synergy on deinking efficiency, and this can be confirmed from the experimental result of embodiment 1, embodiment 6 and embodiment 30.
Claims (8)
1. the deinking process for waste paper that adopts mixed enzyme, comprises the steps:
(1) under temperature is 25～55 DEG C, the condition of pH=7.0～7.5, the deinking agent aqueous solution and waste paper are uniformly mixed, and incorporation time is 5～40 minutes, obtains spent pulp liquors A; Wherein the weight ratio that feeds intake of waste paper and the deinking agent aqueous solution is 100:(300～900); The described deinking agent aqueous solution contains anion surfactant and non-ionic surface active agent, in weight ratio, and waste paper: anion surfactant: non-ionic surface active agent is 100:(0.05～0.15): (0.05～1.0); Described non-ionic surface active agent general molecular formula is RO (CH
2cH
2o)
nh, wherein R is C
10～C
18alkyl, n=3～12; In the described deinking agent aqueous solution, go back cellulase 0.2～0.5u/g, lipase 0.3～1.0u/g and amylase 0.2～1.0u/g;
(2), to thin up in spent pulp liquors A and add acidic ph modifier, obtain taking waste paper weight concentration as 0.6～1.0wt%, the spent pulp liquors B of pH=6.5～6.9;
(3) spent pulp liquors B is carried out to flotation processing and obtain deinking slurries;
The anion surfactant in the anion surfactant that the described anion surfactant of step (1) is originated by soybean oil and cottonseed oil source forms; The anion surfactant in described soybean oil source is at least one in aliphatic acid potassium or the sodium soap in soybean oil source; The anion surfactant in described cottonseed oil source is at least one in aliphatic acid potassium or the sodium soap in cottonseed oil source.
2. deinking process for waste paper according to claim 1, the temperature that it is characterized in that step (1) is 40～50 DEG C.
3. deinking process for waste paper according to claim 1, the pH that it is characterized in that step (1) is 7.2～7.4.
4. want its deinking process for waste paper described in 1 according to right, the incorporation time that it is characterized in that step (1) is 10～20 minutes.
5. deinking process for waste paper according to claim 1, is characterized in that R is C
12～C
14alkyl, n=5～10.
6. deinking process for waste paper according to claim 1, is characterized in that pH adjusting agent described in step (2) is at least one in EDTA Dipotassium salt or disodium EDTA, ethylenediamine tetra-acetic acid di-ammonium salts.
7. deinking process for waste paper according to claim 1, is characterized in that the described pH of step (2) is 6.5～6.8.
8. deinking process for waste paper according to claim 1, is characterized in that the temperature of step (3) flotation is 20～85 DEG C.
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| CN104861764B (en) * | 2014-02-26 | 2020-08-11 | 胡锴 | Technology for removing laser printing or copying handwriting on surface of paper |
| CN107059454B (en) * | 2017-05-08 | 2018-05-15 | 南京林业大学 | A kind of method that deinking is carried out using bifunctional fusion enzyme Lip-EG1CD |
| CN109208367A (en) * | 2018-09-30 | 2019-01-15 | 兰溪泛仕达新材料科技有限公司 | A kind of novel waste paper floatation and ink removing agent |
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| CN1331742C (en) * | 2004-03-29 | 2007-08-15 | 同济大学 | Method for synthesizing ultramicro materials of spherica carbonate of alkaline earth controlled through supported liquid membrane |
| CN1312353C (en) * | 2004-11-24 | 2007-04-25 | 深圳市绿微康生物工程有限公司 | New process for lipase waste paper deinking |
| US9587350B2 (en) * | 2010-02-12 | 2017-03-07 | Kemira Oyj | Method for removing ink from paper |
| CN102517949B (en) * | 2011-12-08 | 2013-12-18 | 东莞市绿微康生物科技有限公司 | Environmentally friendly waste paper deinking method |
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