CN103193930B - A kind of preparation method improving the amphiprotic polyacrylamide emulsion of waste paper fine fiber strength - Google Patents
A kind of preparation method improving the amphiprotic polyacrylamide emulsion of waste paper fine fiber strength Download PDFInfo
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- CN103193930B CN103193930B CN201310075603.3A CN201310075603A CN103193930B CN 103193930 B CN103193930 B CN 103193930B CN 201310075603 A CN201310075603 A CN 201310075603A CN 103193930 B CN103193930 B CN 103193930B
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Abstract
The invention discloses a kind of preparation method improving the amphiprotic polyacrylamide emulsion of waste paper fine fiber strength, comprise the following steps: weigh monomer, sodium bisulfite, Potassium Persulphate, polyvinylpyrrolidone, Resorcinol; Described monomer is made up of AM, AMPS and DMC; Monomer is made into monomer solution, and regulates pH value to 3 ~ 4; (3) add ammoniumsulphate soln, polyvinylpyrrolidone, sodium bisulfite in a kettle., pass into nitrogen, after stirring under the condition of 30 ~ 40 DEG C, add Potassium Persulphate, then monomer solution is added dropwise in reactor and carries out polyreaction; (4) after monomer solution all adds, control temperature of reaction at 35 DEG C ~ 40 DEG C, add Resorcinol after reaction terminating and inhibit and stop test operation.Emulsion prepared by the present invention can improve fine fiber strength, good stability and also do not need dissolve, easy to use, product and preparation technology environmentally friendly.
Description
Technical field
The present invention relates to papermaking Slag recovering and utilize field, particularly a kind of preparation method improving the amphiprotic polyacrylamide emulsion of waste paper fine fiber strength.
Background technology
China adopted waste paper to be that raw pulp proportion increases year by year in recent years, according to investigations, the regenerated papermaking proportion of 05 year to 10 years rises to 62.7% by 54.0%, particularly promulgated the raw material policy of " progressively being formed based on xylon, waste paper; non-wood fiber is auxiliary raw material mix " in country after, this trend is further obvious.Waste paper is back to production as paper making raw material, the usage quantity of thallophyta fibrous material can be greatly reduced.But the art breading of pulping making beating in waste paper fibre reuse process, can produce a large amount of fiber fines, and can run off with paper waste at paper-making process, its intensity difference, drainability are poor, is adsorbed with a large amount of anionic trash that paper-making process produces simultaneously.Interference can be produced to paper making wet part at the total anionic trash of the process of copy paper, have a strong impact on manufacturing paper with pulp and quality of finished paper of paper.
Fiber fines cationic demand than the height of waste paper pulp fiber, probably at 11 μm of about oL/g; Zeta potential is-65.13mv; Its specific surface area can reach 500m2g
-1, therefore fiber surface ionizable go out more carboxyl, cause fiber surface electric density to improve, this just causes the high result of Zeta potential absolute value jointly with the anionic trash be present in slurry.Such fiber fines is used for reuse papermaking, first the low problem of its retention will be solved, then its larger cationic demand should also be met, increase its interfibrous bonded area and bonding strength, also quantity and the intensity of hydrogen bonded between its fiber is namely increased, and strengthen original hydrogen bonded, thus increase the intensity of fiber fines.
Have in good water miscible amphiprotic polyacrylamide (AmPAM) molecule simultaneously containing positive and negative charge groups; its anionic group contained shields to cation group; can repel " impurity anions " that exist in residue, thus make cation group react prematurely or to be neutralized.And anionic group can positively charged ion in absorption system, makes cationic auxiliary from assorted cationic interference, can meet the cationic demand that fiber fines is a large amount of, and make the hydrogen bond quantity on the surface of fiber fines increase.Its retention aid and filter aid effect and enhancement are better than and are used alone CPAM or APAM, can meet the requirement of fiber fines reuse papermaking.
The paper making additive being specifically applied to the utilization of papermaking Slag recovering is at present also few, and someone adopts reverse microemulsion process to synthesize AmPAM, shows enhancing and retention and drainage effect for residue result.But, adopt amphiprotic polyacrylamide the product often many and poor stability of impurity of reverse microemulsion process synthesis; If make powder, just need to dissolve more than 1h in advance, not only need large-scale dissolver but also expend the energy, if dissolve insufficient, there will be the insolubles of " flake " shape, not only cause the waste of product, also can cause the decline of application performance.And reverse microemulsion process synthesis need adopt emulsifying agent and varsol, can cause secondary pollution to environment.Given this, develop a kind of economic green, have the paper making additive of comparatively strong enhancing and retention and drainage effect just to seem particularly important to process papermaking residue.
Summary of the invention
The object of the invention is to provide double-aqueous phase polymerization to prepare the method for amphiprotic polyacrylamide emulsion, overcomes that impurity in products in existing amphiprotic polyacrylamide technology of preparing is many, poor stability, powder need dissolve in advance and expends the energy and containing causing the shortcomings such as the emulsifying agent of secondary pollution and varsol to environment.
Object of the present invention is achieved through the following technical solutions: a kind of preparation method improving the amphiprotic polyacrylamide emulsion of waste paper fine fiber strength, comprise the following steps: (1) weighs material by following mass percent: monomer 30% ~ 35%, sodium bisulfite 0.06% ~ 0.09%, Potassium Persulphate 0.04% ~ 0.06%, polyvinylpyrrolidone 0.8% ~ 1.0%, Resorcinol 0.4% ~ 0.6%; Described monomer is made up of AM (acrylamide), AMPS (2-acrylamido-2-methyl isophthalic acid-propane sulfonic acid) and DMC (MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride);
(2) monomer is made into monomer solution, and adjust ph to 3 ~ 4;
(3) in the temperature control reactor that condensation reflux unit, agitator and logical nitrogen pipe are housed, ammoniumsulphate soln, polyvinylpyrrolidone, sodium bisulfite is added, pass into nitrogen, add Potassium Persulphate after stirring under the condition of 30 DEG C ~ 40 DEG C, then monomer solution is added dropwise in reactor and carries out polyreaction;
(4) after monomer solution all adds, control temperature of reaction at 35 DEG C ~ 40 DEG C, add the also stopped reaction still heating of Resorcinol inhibition after reaction terminating, pass into nitrogen and stirring, the emulsion Room-temperature seal generated is preserved.
The mol ratio of described AMPS and DMC is 1:1, and the amount of substance of AM is 0.7:1 ~ 0.8:1 with the ratio of three kinds of total amount of substances of monomer.
Step (3) described stirring, is specially: stir with the speed of 300 ~ 350rpm.
Step (3) is described to be added dropwise in reactor by monomer solution, is specially: be added dropwise in reactor with the speed of 35mL/h ~ 45mL/h by monomer solution.
The time of described polyreaction is 6h ~ 8h.
Compared with prior art, the present invention has the following advantages and beneficial effect: in (1) the present invention, synthesis is used as the AmPAM emulsion of paper making additive is not adopt conversed phase micro emulsion copolymerization method, but adopts double-aqueous phase polymerization method synthesis amphiprotic polyacrylamide.Double-aqueous phase polymerization is diffuse-aggregate one, the present invention adopts inorganic salt solution as dispersion medium, AM, AMPS and DMC are as monomer, PVP is as dispersion agent, Potassium Persulphate and sodium bisulfite are as redox initiator, and monomer is slowly added dropwise in reactor and carries out being obtained by reacting AmPAM emulsion, product emulsion clear stable, can place preservation more than 3 months and not change.
(2) this emulsion combines the advantage of double-aqueous phase polymerization method and amphiprotic polyacrylamide, and the polyacrylamide emulsion of generation, owing to being both sexes, simultaneously containing positive and negative charge groups in molecule, has good water-soluble.The retention aid and filter aid effect of amphiprotic polyacrylamide and enhancement are better than and are used alone cationic polyacrylamide or anionic polyacrylamide; because anionic group shields to cation group; can repel " impurity anions " that exist in residue, thus make cation group react prematurely or to be neutralized.And anionic group can positively charged ion in absorption system, makes cationic auxiliary from assorted cationic interference.And adopt double-aqueous phase polymerization method, product emulsion good stability and do not need to dissolve, easy to use.Its synthesis technique can not produce secondary pollution, and energy consumption is low, the nontoxic non-corrosiveness of product, environmentally friendly.
(3) both sexes synthesized by the present invention gather propionic acid amide emulsion and are used as paper making additive, can significantly improve drainability and the fibre strength of sediment in paper waste, and consumption is only the half of other usual auxiliaries, and price are low.Product is milky white transparence, and median size is 68nm, and particle size range is 60-75nm, and copolymer product intrinsic viscosity is 115.48mL/g, and molecular weight is 30.36 ten thousand, is suitable as paper making additive.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
Mixed with mol ratio AM:AMPS:DMC=70:15:15 by three kinds of monomers, quality is 60g, accounts for 30% of total mass, adds suitable quantity of water and dissolves and regulator solution pH value to 3, and add 0.12g reductive agent sodium bisulfite.
Condensation reflux unit is being housed, the aqueous solution containing 45g ammonium sulfate and 1.6g polyvinylpyrrolidone is added in the reactor of agitator, thermometer and logical nitrogen pipe, while the mixing solutions in reactor is stirred with the speed of 300r/min while be heated to 35 DEG C, add 0.08g oxidizing initiators Potassium Persulphate, pass into nitrogen.
Monomer solution is added dropwise in reactor with the speed of 35mL/h, under air-proof condition, reacts 6h, after reaction terminates, stop heating, logical nitrogen and stirring, emulsion will be generated and take out.Add 0.008g hydroquinone of polymerization retarder Room-temperature seal to preserve.
The amphiprotic polyacrylamide emulsion adopting the present embodiment to prepare is tested as paper making additive, and the result obtained is as shown in table 1.
Amphiprotic polyacrylamide emulsion prepared by table 1. the present embodiment joins the enhancement of copying sediment mixed pulp to OCC paper waste
Slurry is sediment from certain secondary corrugating material papermill whitewater section and secondary corrugating material magma, its sediment is Dark grey mud shape, need first to remove moisture through sludge tank, then partial impurities is removed through vanning, by taper sand cleaning machine, papermaking sediment is removed part of ash again, then obtain purer fiber by Air-sparged hydrocyclone separation and purification.The joining of OCC paper waste and purified sediment fiber copying mass ratio is 7:3, as known from Table 1, when amphiprotic polyacrylamide consumption prepared by the present embodiment is 0.3%, paper basis weight improves 3.0%, tear index improves 15.1%, burst index improves 17.2%, and tensile index improves 7.7%.
Use same slurry, add amphiprotic polyacrylamide emulsion auxiliary agent and other several frequently seen auxiliary agents prepared by the present embodiment, treatment effect is in table 2.
The different paper making additive of table 2 joins the enhancement of copying sediment mixed pulp to OCC paper waste
As known from Table 2, the amphiprotic polyacrylamide emulsion prepared of the present embodiment is compared with existing paper making additive on the market, consumption is few and can reach better enhancing and retention and drainage effect, effectively can solve the problem of the paper strength difference that sediment fiber produces for papermaking.
Embodiment 2
Mixed with mol ratio AM:AMPS:DMC=80:10:10 by three kinds of monomers, quality is 70g, accounts for 35% of total mass, adds suitable quantity of water and dissolves and regulator solution pH value to 4, and add 0.18g reductive agent sodium bisulfite.
Condensation reflux unit is being housed, the aqueous solution containing 40g ammonium sulfate and 2g polyvinylpyrrolidone is added in the reactor of agitator, thermometer and logical nitrogen pipe, while the mixing solutions in reactor is stirred with the speed of 350r/min while be heated to 40 DEG C, add 0.12g oxidizing initiators Potassium Persulphate, pass into nitrogen.
Monomer solution is added dropwise in reactor with the speed of 45mL/h, under air-proof condition, reacts 8h, after reaction terminates, stop heating, logical nitrogen and stirring, emulsion will be generated and take out.Add 0.012g hydroquinone of polymerization retarder Room-temperature seal to preserve.
Embodiment 3
Mixed with mol ratio AM:AMPS:DMC=78:11:11 by three kinds of monomers, quality is 64g, accounts for 32% of total mass, adds suitable quantity of water and dissolves and regulator solution pH value to 3, and add 0.15g reductive agent sodium bisulfite.
Condensation reflux unit is being housed, the aqueous solution containing 46g ammonium sulfate and 1.8g polyvinylpyrrolidone is added in the four-hole boiling flask of agitator, thermometer and logical nitrogen pipe, while the mixing solutions in reactor is stirred with the speed of 320r/min while be heated to 38 DEG C, add 0.1g oxidizing initiators Potassium Persulphate, pass into nitrogen.
Monomer solution is added dropwise in reactor with the speed of 40mL/h, under air-proof condition, reacts 7h, after reaction terminates, stop heating, logical nitrogen and stirring, emulsion will be generated and take out.Add 0.01g hydroquinone of polymerization retarder Room-temperature seal to preserve.
Cost analysis
Amphiprotic polyacrylamide emulsion prepared by the present invention as the cost analysis of auxiliary agent process one ton of paper waste (OCC slurry and sediment fiber) in table 3.
Amphiprotic polyacrylamide emulsion process paper waste per ton (calculating with oven dry stock) cost analysis prepared by table 3 the present invention
Adopt the amphiprotic polyacrylamide emulsion auxiliary agent prepared of the present invention and other conventional paper making additives for the treatment of the Cost comparisons of one ton of fiber fines in table 4.
The cost analysis of the different paper making additive process of table 4 one ton of fiber fines
As seen from the results in Table 4, amphiprotic polyacrylamide emulsion prepared by the present invention effect compared with paper making additive conventional is in the market good, is applied to the reuse of fiber fines, to the water filtering performance of fiber, resident performance, becomes paper dry strength to have significant lifting.And the emulsion of synthesis is not containing the composition of environmental pollution, can not cause secondary pollution to environment, meet at present for the requirement of paper making additive clean and effective.Consumption is relatively few, and cost is low, has good economy, environmental and social benefits, has wide market using value.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not limited by the examples; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. improve a preparation method for the amphiprotic polyacrylamide emulsion of waste paper fine fiber strength, it is characterized in that, comprise the following steps:
(1) material is weighed by following mass percent: monomer 30% ~ 35%, sodium bisulfite 0.06% ~ 0.09%, Potassium Persulphate 0.04% ~ 0.06%, polyvinylpyrrolidone 0.8% ~ 1.0%, Resorcinol 0.4% ~ 0.6%; Described monomer is made up of AM, AMPS and DMC;
(2) monomer is made into monomer solution, and adjust ph to 3 ~ 4;
(3) in the temperature control reactor that condensation reflux unit, agitator and logical nitrogen pipe are housed, ammoniumsulphate soln, polyvinylpyrrolidone, sodium bisulfite is added, pass into nitrogen, add Potassium Persulphate after stirring under the condition of 30 ~ 40 DEG C, then monomer solution is added dropwise in reactor and carries out polyreaction;
(4) after monomer solution all adds, control temperature of reaction at 35 DEG C ~ 40 DEG C, add the also stopped reaction still heating of Resorcinol inhibition after reaction terminating, pass into nitrogen and stirring, the emulsion Room-temperature seal generated is preserved.
2. the preparation method of the amphiprotic polyacrylamide emulsion of raising waste paper fine fiber strength according to claim 1, it is characterized in that, the mol ratio of described AMPS and DMC is 1:1, and the amount of substance of AM is 0.7:1 ~ 0.8:1 with the ratio of three kinds of total amount of substances of monomer.
3. the preparation method of the amphiprotic polyacrylamide emulsion of raising waste paper fine fiber strength according to claim 1, is characterized in that, step (3) described stirring, is specially: stir with the speed of 300 ~ 350rpm.
4. the preparation method of the amphiprotic polyacrylamide emulsion of raising waste paper fine fiber strength according to claim 1, is characterized in that, step (3) is described to be added dropwise in reactor by monomer solution, is specially:
Monomer solution is added dropwise in reactor with the speed of 35mL/h ~ 45mL/h.
5. the preparation method of the amphiprotic polyacrylamide emulsion of raising waste paper fine fiber strength according to claim 1, is characterized in that, the time of described polyreaction is 6h ~ 8h.
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| CN107779183B (en) * | 2017-03-23 | 2020-03-27 | 西南石油大学 | Well cementation cement slurry large temperature difference retarder and preparation method thereof |
| CN108083614B (en) * | 2018-02-05 | 2020-12-08 | 中国科学院长春应用化学研究所 | Water-dispersible diatomite composite flocculation dehydrating agent and application thereof |
| CN110407974B (en) * | 2019-08-15 | 2021-09-21 | 浙江传化华洋化工有限公司 | Preparation method of crosslinkable amphoteric polyacrylamide polymer |
| CN113912771A (en) * | 2021-09-28 | 2022-01-11 | 苏州派凯姆新能源科技有限公司 | Preparation method and application of amphoteric polyacrylamide resin papermaking reinforcing agent |
| CN114108356B (en) * | 2021-10-21 | 2024-05-24 | 江苏理文造纸有限公司 | Papermaking white water anion garbage recycling process |
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| WO2005100423A1 (en) * | 2004-04-07 | 2005-10-27 | Snf Sas | Novel high molecular weight associative amphoteric polymers and uses thereof |
| CN101514239A (en) * | 2008-12-30 | 2009-08-26 | 上海东升新材料有限公司 | Amphoteric polyacrylamide and preparation method thereof |
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