CN102080342B - Anionic organic particles and preparation and application thereof - Google Patents
Anionic organic particles and preparation and application thereof Download PDFInfo
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Abstract
The invention relates to anionic organic particles for a microparticle retention and drainage aid system, preparation and application thereof. The preparation of the anionic organic particles comprises the steps of: preparing nano-microcrystalline cellulose by an acid hydrolysis method or a bioenzyme hydrolysis method by taking wood pulp, microcrystalline cellulose or cotton as a raw material; preparing nano-microcrystalline cellulose suspension into 1 to 10 mass percent of solution B; and then preparing solution A of an anionic modified reagent with the pH value of between 11 and 14 and the concentration of between 1 and 1 percent, mixing the solution A and the solution B according to the proportion, and dialyzing to obtain anion-modified nano-microcrystalline cellulose suspension. 0.05 to 2.0 percent of the anionic organic particles are added to make paper when the anionic organic particles are applied in the microparticle retention and drainage aid system. The anionic organic particles for the microparticle retention and drainage aid system have the characteristics of good biocompatibility and biodegradability, large specific surface area, high surface negative charge density, and good retention and drainage aid effect.
Description
(1) technical field
The present invention relates to a kind of anionic organic particles for papermaking microparticle retention and drainage system and preparation and application method thereof, belong to the pulping and paper-making field.
(2) background technology
China's paper industry is constantly towards high speed, serialization, maximization future development, and this retention aid and filtering aid technology to wet end of machine is had higher requirement.The microparticle retention and drainage system is shown one's talent with its unique advantage.Traditional Microparticle Retention System comprises the Compozil system that is comprised of cataloid and cationic starch, the Hydrocal system that is comprised of modified alta-mud and cationic polyacrylamide, and the cationic starch that occurred afterwards/aluminium hydroxide system.Its application is to apply first macromolecule cation polymer in slurry, poly-by the wadding of building bridge, add again the king-sized electronegative inorganic matter of special specific area, by electrochemical action and the positive charge patch that forms at fiber fines and fiber surface crosslinked little wadding polymers that makes it to form occurs.Although traditional microparticle retention system is widely used, the exploitation of microparticle system Research on the effect mechanism and new microparticle system still is devoted in a large amount of work.The organic fine particles retention aid and filtering aid system receives increasing concern.Organic fine particles has controlled charge density and function base, has again the 3-D nano, structure of inorganic particles simultaneously, becomes more effective particulate constituent in the microparticle retention and drainage system.
The non-renewable resources such as current coal, oil and natural gas are day by day exhausted, and the development and use renewable resource becomes inexorable trend.Natural fabric as one of renewable resource is a kind of material that is formed by self compounding, and it not only has biodegradability, and is the widest boiomacromolecule of occurring in nature distribution.Potential performance, the new fine chemical product of exploitation take native cellulose as raw material of fully excavating natural fabric will be one of important topics of 21 century sustainable development Chemical Engineering research field.
Acid hydrolysis or cellulose hydrolyzation cellulose fibre can access nano micro crystal cellulose (nanocrystalline cellulose, NCC), and this has further enlarged the use of cellulose at Material Field.NCC and the polymer that be easy to degrade relatively cheap as, its major advantage comprise biological degradability, biocompatibility, avirulence, DIMENSIONAL STABILITY, high strength, lightweight, durability, high-hygroscopicity, are easy to carry out chemistry and physical modification.Nano micro crystal cellulose has nano-scale, and larger specific area can be used as the anionic organic particles in the microparticle retention and drainage system, and after its surface modification, the negative charge amount on surface increases, and stability increases, and its retention and drainage effect is more obvious.
(3) summary of the invention
The invention provides a kind of anionic organic particles and preparation and application thereof for papermaking microparticle retention and drainage system.
Organic anion particulate of the present invention is by acid treatment or cellulase treatment plant fiber material or paper pulp, obtain nano micro crystal cellulose, then nano micro crystal cellulose is carried out anion-modified obtaining.
Technical scheme of the present invention is as follows:
A kind of anionic organic particles for papermaking microparticle retention and drainage system is prepared by following methods:
(1) take deinking of MOW slurry, bleaching softwood kraft pulp, bleaching broad-leaved wood sulphate pulp, microcrystalline cellulose (MCC) or cotton as raw material, adopt one of following method preparation nano micro crystal cellulose:
Acid-hydrolysis method:
Raw material is smashed, crossed 20 mesh sieves, at 20 ℃-65 ℃ lower hydrochloric acid or the 30-64wt% sulfuric acid that add concentration 30-64wt%, the volume mass that makes acid and raw material is than (5～15): 1, and unit milliliter Bick, former slip is in the over dry material; Under stirring, then reaction 10-70min dilutes 10 times of cessation reactions with suspension with deionized water.Product with deionized water repeatedly centrifugal elutriation to pH value 5.0～5.5.To obtain product and put into bag filter, dialyse to constant pH with the deionized water that flows.Suspension after the dialysis carries out supersonic oscillations and processes 5-50min in ice-water bath.For avoiding product because of the hot polymerization collection, ultrasonic oscillator is processed and is carried out in ice-water bath.Obtain nano micro crystal cellulose suspension.Perhaps,
The biological enzyme hydrolysis method:
Raw material is pulverized, cross 20 mesh sieves, the raw material of getting after the pulverizing is put into conical flask, adds entry in conical flask, adds the pH value of buffer solution regulator solution to 6-7 again, add cellulase, every gram over dry raw material adds cellulase 5000～80000IU, places shaking table, and temperature regulating is to 40-60 ℃, hunting speed is 50-250r/min, and reaction 24-72h makes cellulose generation enzymolysis.After reaction finishes, take out sample, centrifugation obtains Nanocrystalline Cellulose Colloid suspension.
Described cellulase is the neutral cellulase that jade of the He family Bioisystech Co., Ltd produces, its filter paper enzyme activity 20000～40000IU/g.
(2) the anion-modified reagent solution of mass concentration 1-10% being transferred to pH value 11-14 is solution A, and described anion-modified reagent is boric acid, phenyl boric acid, Boratex or potassium borate.
(3) the nano micro crystal cellulose suspension that step (1) is made is configured to the solution B of mass concentration 1-10%, then, the solution A that step (2) is made and described solution B are by (9～1): 1 volume ratio is mixed, after 10-100r/min slow speed lower magnetic force stirs 1-30min, dialysis is 5-10 days in the deionized water that flows, obtain anion-modified nano micro crystal cellulose suspension, be the anionic organic particles for papermaking microparticle retention and drainage system.
Above-mentioned anion-modified reagent is boric acid, phenyl boric acid, Boratex or potassium borate.
Preferably, buffer solution is phosphate buffered solution described in above-mentioned steps (1) the biological enzyme hydrolysis method, gets sodium dihydrogen phosphate 1.74g, sodium hydrogen phosphate 2.7g, and sodium chloride 1.7g, the solution preparation that is dissolved in water into 400ml forms.
Preferably, the bag filter molecular cut off that uses in above-mentioned steps (1) acid-hydrolysis method is 12000-14000.
Preferably, state that anion-modified reagent is boric acid or phenyl boric acid in the step (2), concentration of polymer solution is 4-6%.
Preferably, solution A is pressed (5～3) with solution B in the above-mentioned steps (3): 1 volume ratio is mixed.
Preferably, the bag filter molecular cut off that dialysis is used in the above-mentioned steps (3) is 12000-14000.
The application of anionic organic particles of the present invention in papermaking microparticle retention and drainage system, method is as follows:
In the paper stock of mass concentration 0.1%-1%, percentage by weight by relative over dry paper stock adds 5%-30% filler, 1.0%-3% sizing agent, mixing speed 700-750rpm condition adds the high-molecular cationic polymer of 0.01%-2%, after mixing 1min-10min, improve the mixing speed of paper stock system to 1200-1500rpm, keep recovering the mixing speed of system to 700-750rpm behind the 30s-5min, the anionic organic particles of the present invention that adds 0.05%-2.0% is copied into paper behind the effect 30s-5min.Above percentage all is the percentage of relative over dry paper stock weight.
Above-mentioned macromolecule cation polymer is cationic starch, cationic polyacrylamide or cationic starch grafted polyacrylamide.Be this area raw material commonly used, market is on sale.
Above-mentioned filler is calcium carbonate or talcum powder, and sizing agent is gum rosin, alkyl ketene dimer (AKD) or alkenyl succinic anhydride (ASA).Be this area typical additives, market is on sale.
Technical characterstic of the present invention and excellent results are as follows:
Paper industry is faced with huge resource and environment pressure, with the standby papermaking chemical product of biomass-making and utilize living resources to carry out the biological and chemical modification to prepare new material, be the direction that following paper already develops.The present invention utilizes the widest cellulose of distributed in nature for the preparation of the anionic organic particles of papermaking microparticle retention and drainage system, has good biocompatibility and biodegradability.Its size is in nanometer range, and specific area is large, and surperficial negative charge density is high, and as the anionic organic particles in the microparticle retention and drainage system, retention and drainage effect is good.
(4) specific embodiment
The present invention will be further described below in conjunction with specific embodiment, but be not limited to this.
Embodiment 1:
(1) with pulverizer bleached hardwood pulp is pulverized, crossed 20 mesh sieves, 20g gets in the over dry slurry.(wintercherry is than 8.5, ml/g) and mix, reacts under mechanical agitation, and reaction 30min comes cessation reaction with suspension with 10 times of deionized water dilutions after the time to add the sulfuric acid 170ml of mass concentration 64% under 45 ℃.Product with deionized water repeatedly centrifugal elutriation to pH value be 5.0.Product after centrifugal is put into bag filter (molecular cut off 12000-14000), dialyse some days to constant pH with the deionized water that flows.Suspension after the dialysis is processed 10min with ultrasonic oscillator, for avoiding product because of the hot polymerization collection, processes and carries out in ice-water bath.
(2) BAS with mass concentration 5% transfers to pH value 13, is solution A 1.
(3) the nano micro crystal cellulose suspension that step (1) is made is configured to the solution B 1 of mass concentration 4%, then solution A 1 and solution B 1 is mixed in 5: 1 by volume.After slow speed 30r/min lower magnetic force stirs 10min, obtain anion-modified nano micro crystal cellulose.
Use:
Be to add 20% calcium carbonate and 1% anion gum rosin in 0.3% the bleaching waste newspaper deinking pulp in mass concentration, mix the cationic starch of rear adding 0.05% under the 750rpm rotating speed, behind the effect 30s rotating speed is increased to 1500rpm, behind the effect 1min rotating speed is down to 750rpm, then add the anion-modified nano micro crystal cellulose that 0.5% above-mentioned steps (3) makes, after mixing 1min paper stock is copied into paper, the retention 92% of paper stock after dry, and the drainage rate of paper stock is fast, and paper-forming evenness is good.The percentage of above additive all is the percentage of relative over dry paper stock weight.
Embodiment 2:
(1) accurately takes by weighing MCC 6g and put into conical flask, the water that adds aequum (cumulative volume that makes final mixed liquor is 200ml) in the conical flask, add again the pH value of 2ml buffer solution regulator solution to 6-7, add subsequently cellulase, the cellulase consumption is 20000IU/g over dry raw material, places shaking table, temperature regulating to 50 ℃, hunting speed is 126r/min, and reaction 48h makes cellulose generation enzymolysis.After reaction finishes, take out sample, centrifugation.Get Nanocrystalline Cellulose Colloid suspension.
Used cellulase is that jade of the He family Bioisystech Co., Ltd produces the neutral cellulase of selling, its filter paper enzyme activity 20000～40000IU/g.
(2) BAS with mass concentration 5% transfers to pH value 13, is solution A 2.
(3) the Nanocrystalline Cellulose Colloid suspension that step (1) is made is configured to the solution B 2 of mass concentration 4%, then solution A 2 and solution B 2 were mixed in 5: 1 by volume, after slow speed 50r/min lower magnetic force stirs 10min, obtain anion nano-cellulose crystallite.
Use:
Be to add 20% calcium carbonate and 1% anion gum rosin in 0.3% the bleached chemical thermomechanical pulp in mass concentration, mix the cationic starch of rear adding 0.05% under the 750rpm rotating speed, behind the effect 30s rotating speed is increased to 1500rpm, behind the effect 1min rotating speed is down to 750rpm, then add the anion-modified nano-cellulose crystallite that 0.5% above-mentioned steps (3) makes, after mixing 1min paper stock is copied into paper, the retention 92.5% of paper stock after dry, and the drainage rate of paper stock is fast, and paper-forming evenness is good.The percentage of above additive all is the percentage of relative over dry paper stock weight.
Embodiment 3:
As described in Example 1, difference is that raw material is the bleaching softwood kraft pulp.
Embodiment 4:
As described in Example 1, difference is that raw material is microcrystalline cellulose (MCC).
Embodiment 5
As described in Example 1, difference is to use phenyl boric acid to carry out anion-modified in step (2).
Embodiment 6:
As described in Example 1, difference is to use Boratex to carry out anion-modified in the step (2).
Embodiment 7:
As described in Example 2, difference is that raw material is the bleaching softwood kraft pulp.
Embodiment 8:
As described in Example 2, difference is that raw material is microcrystalline cellulose.
Embodiment 9: as described in Example 2, difference is to use phenyl boric acid to carry out anion-modified in step (2).
Claims (8)
1. anionic organic particles that is used for papermaking microparticle retention and drainage system is prepared by following methods:
(1) take deinking of MOW slurry, bleaching softwood kraft pulp, bleaching broad-leaved wood sulphate pulp, microcrystalline cellulose or cotton as raw material, adopt one of following method preparation nano micro crystal cellulose suspension:
Acid-hydrolysis method:
Raw material is pulverized, crossed 20 mesh sieves, at 20 ℃-65 ℃ lower sulfuric acid that add concentration 30-64wt%, the volume mass that makes acid and raw material is than (5～15): 1, and unit milliliter Bick, former slip is in the over dry material; Under stirring, then reaction 10-70min dilutes 10 times of cessation reactions with suspension with deionized water; Product with deionized water repeatedly centrifugal elutriation to pH value 5.0～5.5; To obtain product and put into bag filter, dialyse to constant pH with the deionized water that flows; Suspension after the dialysis carries out supersonic oscillations and processes 5-50min in ice-water bath, obtain nano micro crystal cellulose suspension; Perhaps,
The biological enzyme hydrolysis method:
Raw material is pulverized, cross 20 mesh sieves, the raw material of getting after the pulverizing is put into conical flask, adds entry in conical flask, adds the pH value of buffer solution regulator solution to 6-7 again, add cellulase, every gram over dry raw material adds cellulase 5000 ~ 80000IU, places shaking table, and temperature regulating is to 40-60 ℃, hunting speed is 50-250r/min, and reaction 24-72h makes cellulose generation enzymolysis; After reaction finishes, take out sample, centrifugation gets Nanocrystalline Cellulose Colloid suspension;
Described cellulase is the neutral cellulase that jade of the He family Bioisystech Co., Ltd produces, its filter paper enzyme activity 20000 ~
40000IU/g；
(2) the anion-modified reagent solution of mass concentration 1-10% being transferred to pH value 11-14 is solution A, and described anion-modified reagent is boric acid, phenyl boric acid, Boratex or potassium borate;
(3) the nano micro crystal cellulose suspension that step (1) is made is configured to the solution B of mass concentration 1-10%, then, the solution A that step (2) is made and described solution B are by (9～1): 1 volume ratio is mixed, after 10-100r/min slow speed lower magnetic force stirs 1-30min, dialysis is 5-10 days in the deionized water that flows, obtain anion-modified nano micro crystal cellulose suspension, be the anionic organic particles for papermaking microparticle retention and drainage system.
2. the anionic organic particles for papermaking microparticle retention and drainage system as claimed in claim 1, it is characterized in that buffer solution is phosphate buffered solution described in step (1) the biological enzyme hydrolysis method, get sodium dihydrogen phosphate 1.74g, sodium hydrogen phosphate 2.7g, sodium chloride 1.7g, the solution preparation that is dissolved in water into 400ml forms.
3. the anionic organic particles for papermaking microparticle retention and drainage system as claimed in claim 1 is characterized in that the bag filter molecular cut off that uses in step (1) acid-hydrolysis method is 12000-14000.
4. the anionic organic particles for papermaking microparticle retention and drainage system as claimed in claim 1 is characterized in that anion-modified reagent is boric acid or phenyl boric acid in the step (2), and concentration of polymer solution is 4-6%.
5. the anionic organic particles for papermaking microparticle retention and drainage system as claimed in claim 1, it is characterized in that solution A is pressed (5～3) with solution B in the step (3): 1 volume ratio is mixed.
6. each described anionic organic particles for papermaking microparticle retention and drainage system of claim 1～5 is in the application of papermaking microparticle retention and drainage system, and method is as follows:
In the paper stock of mass concentration 0.1%-1%, percentage by weight by relative over dry paper stock adds 5%-30% filler, 1.0%-3% sizing agent, mixing speed 700-750rpm condition adds the high-molecular cationic polymer of 0.01%-2%, after mixing 1min-10min, improve the mixing speed of paper stock system to 1200-1500rpm, the mixing speed that keeps recovering system behind the 30s-5min adds the described anionic organic particles of 0.05%-2.0% to 700-750rpm, copies into paper behind the effect 30s-5min; Above percentage all is the percentage of relative over dry paper stock weight;
Above-mentioned macromolecule cation polymer is cationic starch, cationic polyacrylamide or cationic starch grafted polyacrylamide.
7. the anionic organic particles for papermaking microparticle retention and drainage system as claimed in claim 6 is characterized in that in the application of papermaking microparticle retention and drainage system described filler is calcium carbonate or talcum powder.
8. the anionic organic particles for papermaking microparticle retention and drainage system as claimed in claim 6 is characterized in that in the application of papermaking microparticle retention and drainage system described sizing agent is gum rosin, alkyl ketene dimer or alkenyl succinic anhydride.
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| CN103930618B (en) * | 2011-11-14 | 2016-06-08 | 凯米拉公司 | The production of AKD composition and paper and paperboard |
| EP2639351A1 (en) * | 2012-03-13 | 2013-09-18 | Södra Skogsägarna ekonomisk förening | Retention of cellulose fibres |
| ES2384931B1 (en) * | 2012-05-03 | 2013-03-20 | Saica Pack, S.L. | Procedure for obtaining nanodispersed cellulose from recovered paper |
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| KR20150013055A (en) * | 2013-07-26 | 2015-02-04 | 박찬오 | A bio-degradable composition comprising cellulose, a manufacturing method for the same, and a water-proof agnet and goods using the same |
| FI126733B (en) * | 2013-09-27 | 2017-04-28 | Upm Kymmene Corp | Process for the preparation of pulp slurry and paper product |
| CN103588886B (en) * | 2013-11-19 | 2016-08-17 | 武汉理工大学 | A kind of Easily-water dispersible nanocrystalline cellulose and preparation method thereof |
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| CN104532645B (en) * | 2014-11-11 | 2016-06-29 | 浙江理工大学 | A kind of method preparing nano micro crystal cellulose for raw material with waste and old corrugated board |
| CN105113320A (en) * | 2015-07-08 | 2015-12-02 | 浙江理工大学 | Method for improving strength of wastepaper fibers based on nanometer microcrystalline cellulose |
| CN107513879B (en) * | 2017-10-23 | 2019-11-05 | 南京林业大学 | A kind of recycling reuse method of mthod of white water from paper making anionic trash |
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