CN105037605A - AOS-AA biopolymer surfactant and preparation method and application thereof - Google Patents
AOS-AA biopolymer surfactant and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides an AOS-AA biopolymer surfactant and a preparation method and application thereof. The AOS-AA biopolymer surfactant is formed by polymerization reaction of monomer alpha-alkene sodium sulfonate and monomer crylic acid under the action of ammonium persulfate as an initiator, wherein molar ratio of the monomer alpha-alkene sodium sulfonate to monomer crylic acid is 1: (1-4), usage amount of the initiator accounts for the monomer total mass by 0.5-4.5%, a reaction medium is water, mass percent concentration of the alpha-alkene sodium sulfonate in the reaction system is 10-15%. Compared with a commercially available low molecular deinking agent, the AOS-AA biopolymer surfactant has larger molecular mass, higher dispersing, capturing and emulsifying capacity for printing ink, can be singly used or compounded with a low molecular surfactant as a deinking agent for waste paper deinking, regenerated white paper has high whiteness, residual ink is less, and the AOS-AA biopolymer surfactant is particularly suitable for floating deinking of waste magazine paper and has well application prospect.
Description
Technical field
The invention belongs to deinking technical field, relate to a kind of tensio-active agent that can be used for deinking, particularly a kind of AOS-AA copolymer tensio-active agent and its preparation method and application.
Background technology
Nowadays, world environments constantly worsens, wood raw material supply wretched insufficiency.13% of the total area of woods in the area of woods Jin Zhan world of China, and per capita rate is only 15% of world's per capita share, but our paper using demand is but in continuous increase, so this just needs us to strengthen use to recycled writing paper.Deinking is the important channel of waste paper second stage employ, and its gordian technique is exactly the Study and Development of deinking agent.
Though current domestic waste paper deinking agent is wide in variety, its intrinsic chemical product are substantially identical, mostly are the single or composite use of low-molecular-weight surfactant.But the development of synthetic resins causes the kind of ink constantly to increase, and existing deinking agent can not meet the demand in market, so it is imperative to develop deinking agent that is novel, efficient, applied range.
Copolymer surfactants due to its structure special, the huge number that can synthesize, and the performances such as its dispersion, emulsification, steady bubble all strengthen to some extent than low-molecular-weight surfactant.But the research of current related copolymers deinking agent is few.Multipolymer deinking agent can not only be used alone, and all right and composite use of low molecule deinking agent, both can carry out performance complement, improve deinking efficiency better, so it has wide development and application prospect.
Summary of the invention
The object of the present invention is to provide a kind of AOS-AA copolymer tensio-active agent and its preparation method and application, the method is simple, and obtained AOS-AA copolymer tensio-active agent has good deinking efficiency.
For achieving the above object, the technical solution used in the present invention is:
A kind of AOS-AA copolymer tensio-active agent, this AOS-AA copolymer tensio-active agent is generated by polyreaction under the effect of initiator ammonium persulfate by monomer alpha-olefin sodium sulfonate (AOS) and monomeric acrylic (AA), wherein alpha-olefin sodium sulfonate and acrylic acid mol ratio are 1:(1-4), initiator amount is 0.5 ~ 4.5% of monomer total mass, reaction medium is water, and in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 10 ~ 15%.
A preparation method for AOS-AA copolymer tensio-active agent according to claim 1, concrete steps are as follows:
Monomer alpha-olefin sodium sulfonate, monomeric acrylic, initiator ammonium persulfate and water are joined in the isothermal reaction container of 65 ~ 105 DEG C, insulation reaction 2 ~ 7h, leave standstill after reaction terminates, naturally cool to room temperature, then adjust ph to 8 ~ 9, namely obtain AOS-AA copolymer tensio-active agent.
Described monomer alpha-olefin sodium sulfonate and monomeric acrylic feed intake at twice, and each input monomer alpha-olefin sodium sulfonate of half and the monomeric acrylic of half, the interval time fed intake for twice is 50 ~ 60min.
Described initiator ammonium persulfate takes the mode dripped to feed intake, start to drip initiator continuously when first time drops into monomer alpha-olefin sodium sulfonate and monomeric acrylic, the dropping used time of initiator is 80 ~ 90min, carries out insulation reaction again after dripping initiator.
With the speed of 25 ~ 30r/min, reaction system is stirred in the process dripping initiator.
Speed with 50 ~ 60r/min in insulation reaction process stirs reaction system.
Described monomer alpha-olefin sodium sulfonate first filters before use and removes impurity, then regulates its pH value to neutral.
By the NaOH solution adjust ph that massfraction is 15 ~ 25%.
Described AOS-AA copolymer tensio-active agent is as the application of deinking agent in deinking.
The application in deinking agent prepared by described AOS-AA copolymer tensio-active agent.
Relative to prior art, beneficial effect of the present invention is:
AOS-AA copolymer tensio-active agent prepared by the present invention is compared with commercially available low molecule deinking agent, its molecular chain is longer, molecular weight is larger, to the dispersion of ink, trapping, emulsification and washability stronger, not only can carry out deinking as deinking agent separately, deinking efficiency is good, the Paper White Degree born again is high, residual ink is few, but also can carry out composite with commercially available low molecule deinking agent, for the preparation of deinking agent waste paper being carried out to deinking, by the synergy of AOS-AA copolymer tensio-active agent and commercially available low molecule deinking agent, composite deinking agent is made to have better deinking efficiency, recycled paper whiteness is high, residual ink is few, be specially adapted to the floatation and ink removing of waste and old magazine paper, therefore AOS-AA copolymer tensio-active agent provided by the invention has a good application prospect.
The preparation method of AOS-AA copolymer tensio-active agent provided by the invention is simple, raw material is easy to get, and preparation cost is lower, and preparation cycle is short, and temperature of reaction is low, and required conversion unit is simply common, is easy to suitability for industrialized production.
Further, because the double bond of alpha-olefin sodium sulfonate is not on end position, more difficultly carry out polyreaction, and vinylformic acid is very easy to carry out autohemagglutination, therefore alpha-olefin sodium sulfonate and vinylformic acid are fed intake at twice, and lasting for initiator is added dropwise in reaction system, the polymerization difficulty of alpha-olefin sodium sulfonate can be reduced like this, reduce acrylic acid autohemagglutination phenomenon, improve the productive rate of target product.
Embodiment
Below the present invention is further elaborated.
The preparation method of AOS-AA copolymer tensio-active agent provided by the invention, its reaction principle is as follows:
Obtained AOS-AA copolymer tensio-active agent is tested, finds that the ratio of m, the n in above-mentioned molecular formula is about 1:(1 ~ 4).
Be described in further detail with the preparation method of specific embodiment to AOS-AA copolymer tensio-active agent of the present invention below.
Embodiment 1:
Reaction raw materials: mol ratio be the monomer alpha-olefin sodium sulfonate of 1:1 and monomeric acrylic, monomer total mass 3.0% initiator ammonium persulfate, surplus is deionized water (reaction medium), and wherein in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 12%.
Step: first monomer alpha-olefin sodium sulfonate is crossed and filter impurity, and be adjusted to neutrality by the NaOH solution that massfraction is 20%, again using deionized water as reaction medium, by deionized water, the monomer alpha-olefin sodium sulfonate (AOS) of half and the monomeric acrylic (AA) of half drop in the there-necked flask of 85 DEG C, AOS and AA of remainder is added again after 1h, and just start to continue slowly initiator ammonium persulfate to be added dropwise in there-necked flask after AOS and AA is added there-necked flask by first time, time for adding is 1.5h, speed with 25r/min in dropping process stirs reaction system.Dropwise rear constant temperature and continue reaction 4h, speed with 55r/min in insulation reaction process stirs reaction system, leave standstill after question response terminates, naturally cool to room temperature, then pH is regulated to be 8.5 by the NaOH solution that massfraction is 20%, finally the solid content amber transparent liquid that is about 20% is AOS-AA copolymer tensio-active agent, be designated as deinking agent-1.
Examination of infrared spectrum is carried out to obtained deinking agent-1, the major absorbance peak in its infrared spectrogram and being attributed to:
3400cm
-1place is the association absorption peak of-OH on the-OH on carboxyl and a small amount of water molecules, 2925cm
-1and 2857cm
-1place is respectively antisymmetric stretching vibration peak and the symmetrical stretching vibration peak of C-H, 1644cm
-1place is the stretching vibration peak of C=C, 1572cm
-1and 1411cm
-1place is respectively the stretching vibration peak of carboxylate salt C=O and the stretching vibration peak of C-O, 1457cm
-1place is the in-plane bending stretching vibration peak of C-H, 1193cm
-1and 1062cm
-1place is respectively antisymmetric stretching vibration peak and the stretching vibration peak of sulfonic group S=O, at 1640cm
-1the peak at place is not obvious, illustrates that polyreaction occurs.Summary analysis is bright, has sulfonic group, carboxyl etc. in the molecular structure of this tensio-active agent.
Carry out gel permeation chromatography (GPC) analysis to obtained deinking agent-1, its molecular chain conformation is:
Molecular-weight average M
n=3513, weight-average molecular weight M
w=3900, viscosity-average molecular weight M
p=4518, Z-average molecular weight M
z=4173, (Z+1)-average molecular weight M
z+1=4377, molecular weight of product dispersion coefficient M
w/ M
n=1.110006.
Can be shown by above infrared spectra and gel osmoticing chromatogram analysis, synthetic product is expection product.
Embodiment 2:
Reaction raw materials: mol ratio be the monomer alpha-olefin sodium sulfonate of 1:2 and monomeric acrylic, monomer total mass 1.5% initiator ammonium persulfate, surplus is deionized water (reaction medium), and wherein in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 12%.
Step: first monomer alpha-olefin sodium sulfonate is crossed and filter impurity, and be adjusted to neutrality by the NaOH solution that massfraction is 20%, again using deionized water as reaction medium, by deionized water, the monomer alpha-olefin sodium sulfonate (AOS) of half and the monomeric acrylic (AA) of half drop in the there-necked flask of 85 DEG C, AOS and AA of remainder is added again after 1h, and just start to continue slowly initiator ammonium persulfate to be added dropwise in there-necked flask after AOS and AA is added there-necked flask by first time, time for adding is 1.5h, speed with 25r/min in dropping process stirs reaction system.Dropwise rear constant temperature and continue reaction 4h, speed with 55r/min in insulation reaction process stirs reaction system, leave standstill after question response terminates, naturally cool to room temperature, then pH is regulated to be 8.5 by the NaOH solution that massfraction is 20%, finally the solid content amber transparent liquid that is about 20% is AOS-AA copolymer tensio-active agent, be designated as deinking agent-2.
Embodiment 3:
Reaction raw materials: mol ratio be the monomer alpha-olefin sodium sulfonate of 1:2 and monomeric acrylic, monomer total mass 3.0% initiator ammonium persulfate, surplus is deionized water (reaction medium), and wherein in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 12%.
Step: first monomer alpha-olefin sodium sulfonate is crossed and filter impurity, and be adjusted to neutrality by the NaOH solution that massfraction is 20%, again using deionized water as reaction medium, by deionized water, the monomer alpha-olefin sodium sulfonate (AOS) of half and the monomeric acrylic (AA) of half drop in the there-necked flask of 85 DEG C, AOS and AA of remainder is added again after 1h, and just start to continue slowly initiator ammonium persulfate to be added dropwise in there-necked flask after AOS and AA is added there-necked flask by first time, time for adding is 1.5h, speed with 25r/min in dropping process stirs reaction system.Dropwise rear constant temperature and continue reaction 4h, speed with 55r/min in insulation reaction process stirs reaction system, leave standstill after question response terminates, naturally cool to room temperature, then pH is regulated to be 8.5 by the NaOH solution that massfraction is 20%, finally the solid content amber transparent liquid that is about 20% is AOS-AA copolymer tensio-active agent, be designated as deinking agent-3.
Embodiment 4
Reaction raw materials: mol ratio be the monomer alpha-olefin sodium sulfonate of 1:3 and monomeric acrylic, monomer total mass 1.0% initiator ammonium persulfate, surplus is deionized water (reaction medium), and wherein in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 10%.
Step: first monomer alpha-olefin sodium sulfonate is crossed and filter impurity, and be adjusted to neutrality by the NaOH solution that massfraction is 20%, again using deionized water as reaction medium, by deionized water, the monomer alpha-olefin sodium sulfonate (AOS) of half and the monomeric acrylic (AA) of half drop in the there-necked flask of 95 DEG C, AOS and AA of remainder is added again after 50min, and just start to continue slowly initiator ammonium persulfate to be added dropwise in there-necked flask after AOS and AA is added there-necked flask by first time, time for adding is 80min, speed with 26r/min in dropping process stirs reaction system.Dropwise rear constant temperature and continue reaction 5h, speed with 50r/min in insulation reaction process stirs reaction system, leave standstill after question response terminates, naturally cool to room temperature, then regulate pH to be 8 by the NaOH solution that massfraction is 20%, finally the solid content amber transparent liquid that is about 20% is AOS-AA copolymer tensio-active agent.
Embodiment 5
Reaction raw materials: mol ratio be the monomer alpha-olefin sodium sulfonate of 1:4 and monomeric acrylic, monomer total mass 4.5% initiator ammonium persulfate, surplus is deionized water (reaction medium), and wherein in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 11%.
Step: first monomer alpha-olefin sodium sulfonate is crossed and filter impurity, and be adjusted to neutrality by the NaOH solution that massfraction is 20%, again using deionized water as reaction medium, by deionized water, the monomer alpha-olefin sodium sulfonate (AOS) of half and the monomeric acrylic (AA) of half drop in the there-necked flask of 105 DEG C, AOS and AA of remainder is added again after 52min, and just start to continue slowly initiator ammonium persulfate to be added dropwise in there-necked flask after AOS and AA is added there-necked flask by first time, time for adding is 82min, speed with 27r/min in dropping process stirs reaction system.Dropwise rear constant temperature and continue reaction 3h, speed with 60r/min in insulation reaction process stirs reaction system, leave standstill after question response terminates, naturally cool to room temperature, then regulate pH to be 9 by the NaOH solution that massfraction is 20%, finally the solid content amber transparent liquid that is about 20% is AOS-AA copolymer tensio-active agent.
Embodiment 6
Reaction raw materials: mol ratio be the monomer alpha-olefin sodium sulfonate of 1:1.5 and monomeric acrylic, monomer total mass 0.4% initiator ammonium persulfate, surplus is deionized water (reaction medium), and wherein in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 13%.
Step: first monomer alpha-olefin sodium sulfonate is crossed and filter impurity, and be adjusted to neutrality by the NaOH solution that massfraction is 20%, again using deionized water as reaction medium, by deionized water, the monomer alpha-olefin sodium sulfonate (AOS) of half and the monomeric acrylic (AA) of half drop in the there-necked flask of 65 DEG C, AOS and AA of remainder is added again after 54min, and just start to continue slowly initiator ammonium persulfate to be added dropwise in there-necked flask after AOS and AA is added there-necked flask by first time, time for adding is 84min, speed with 28r/min in dropping process stirs reaction system.Dropwise rear constant temperature and continue reaction 2h, speed with 52r/min in insulation reaction process stirs reaction system, leave standstill after question response terminates, naturally cool to room temperature, then regulate pH to be 8.2 by the NaOH solution that massfraction is 20%, finally the solid content amber transparent liquid that is about 20% is AOS-AA copolymer tensio-active agent.
Embodiment 7
Reaction raw materials: mol ratio be the monomer alpha-olefin sodium sulfonate of 1:2.5 and monomeric acrylic, monomer total mass 2.0% initiator ammonium persulfate, surplus is deionized water (reaction medium), and wherein in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 14%.
Step: first monomer alpha-olefin sodium sulfonate is crossed and filter impurity, and be adjusted to neutrality by the NaOH solution that massfraction is 20%, again using deionized water as reaction medium, by deionized water, the monomer alpha-olefin sodium sulfonate (AOS) of half and the monomeric acrylic (AA) of half drop in the there-necked flask of 75 DEG C, AOS and AA of remainder is added again after 56min, and just start to continue slowly initiator ammonium persulfate to be added dropwise in there-necked flask after AOS and AA is added there-necked flask by first time, time for adding is 86min, speed with 29r/min in dropping process stirs reaction system.Dropwise rear constant temperature and continue reaction 6h, speed with 58r/min in insulation reaction process stirs reaction system, leave standstill after question response terminates, naturally cool to room temperature, then regulate pH to be 8.8 by the NaOH solution that massfraction is 20%, finally the solid content amber transparent liquid that is about 20% is AOS-AA copolymer tensio-active agent.
Embodiment 8
Reaction raw materials: mol ratio be the monomer alpha-olefin sodium sulfonate of 1:3.5 and monomeric acrylic, monomer total mass 3.5% initiator ammonium persulfate, surplus is deionized water (reaction medium), and wherein in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 15%.
Step: first monomer alpha-olefin sodium sulfonate is crossed and filter impurity, and be adjusted to neutrality by the NaOH solution that massfraction is 20%, again using deionized water as reaction medium, by deionized water, the monomer alpha-olefin sodium sulfonate (AOS) of half and the monomeric acrylic (AA) of half drop in the there-necked flask of 80 DEG C, AOS and AA of remainder is added again after 58min, and just start to continue slowly initiator ammonium persulfate to be added dropwise in there-necked flask after AOS and AA is added there-necked flask by first time, time for adding is 88min, speed with 30r/min in dropping process stirs reaction system.Dropwise rear constant temperature and continue reaction 7h, speed with 56r/min in insulation reaction process stirs reaction system, leave standstill after question response terminates, naturally cool to room temperature, then regulate pH to be 8.7 by the NaOH solution that massfraction is 20%, finally the solid content amber transparent liquid that is about 20% is AOS-AA copolymer tensio-active agent.
Below the deinking efficiency of the AOS-AA copolymer tensio-active agent that the present invention prepares is tested.
Carry out the deinking agent tested:
By AEO-9 (fatty alcohol-polyoxyethylene ether), deinking agent-1, deinking agent-2, deinking agent-3, composite deinking agent-1, composite deinking agent-2, composite deinking agent-3, commercially available deinking agent-1 (XTDM type deinking agent, Qingzhou City Xin Di Chemical Co., Ltd.) and commercially available deinking agent-2 (TM type deinking agent, Tumen City Fangzheng Chemical Aids Plant) individually as deinking agent, carry out deinking experiment.
Wherein, composite deinking agent-1 is in mass ratio for 1:2 obtains after deinking agent-3, AEO-9 mixing; Composite deinking agent-2 is in mass ratio for 1:2:1 obtains after the mixing of deinking agent-3, AEO-9 and commercially available deinking agent-1; Composite deinking agent-3 is in mass ratio for 1:2:1 obtains after the mixing of deinking agent-3, AEO-9 and commercially available deinking agent-2.
Deinking process:
1). waste paper: take 20g and to give up periodical paper, be torn into the fragment of 2cm × 2cm, fully mixes standby whole experimentation and uses.
2). processing parameter: pulping concentration 6%, pulping temperature 60 C, pulping time 30min, curing temperature 60 DEG C, curing time 30min, weaker concn 1.5%.
3). deinking medicine and consumption thereof:
1% of NaOH over dry waste paper quality
NaSiO
33% of over dry waste paper quality
0.2% of deinking agent over dry waste paper quality
4). de-inking method: first added in 60 DEG C of water by above-mentioned deinking medicine, adds the waste paper sheet treating deinking after stirring and dissolving, pulping 30min under certain speed, then slaking 30min is incubated, after slaking terminates, then paper pulp is carried out flotation, handsheet, oven dry successively, handsheet is quantitatively 60 ± 3g/m
-2, detect after drying in the baking oven of 105 ± 3 DEG C.
Deinking result:
The deinking efficiency contrast of AEO-9, deinking agent-1, deinking agent-2, deinking agent-3, composite deinking agent-1, composite deinking agent-2, composite deinking agent-3, commercially available deinking agent-1 and commercially available deinking agent-2 is as shown in table 1.Wherein whiteness adopts YZ-Q-48B type measuring brightness instrument to measure, and ink particle content AutoSpec software measures.
Table 1 deinking efficiency comparing result
The deinking efficiency of deinking agent-3 prepared of the present invention is higher than AEO-9 and commercially available deinking agent as can be seen from Table 1, and the recycled paper whiteness after composite deinking agent-1, composite deinking agent-2 deinking is also higher than by the recycled paper whiteness after AEO-9, commercially available deinking agent-1 and commercially available deinking agent-2 deinking, and the deinking agent-2 prepared with the present invention, deinking agent-3, composite deinking agent-1, paper ink particle content after composite deinking agent-2 deinking are starkly lower than with the ink particle content on paper after AEO-9, commercially available deinking agent-1 and commercially available deinking agent-2 deinking.This is because by the optimization of polymerizing condition, AOS-AA copolymer tensio-active agent provided by the invention its molecular chain compared with commercially available deinking agent is longer, thus has dispersion, emulsification, trapping and washability better to ink.AOS-AA copolymer tensio-active agent not only can be used for deinking as deinking agent separately, and deinking efficiency is good, and Paper White Degree is high, and ink particle content is few.But also composite use can be carried out with commercially available low molecule deinking agent, by the synergy of copolymer surfactants and low-molecular-weight surfactant performance, obtained composite deinking agent has better deinking efficiency, and its recycled paper whiteness is higher, and residual ink is less.Therefore, AOS-AA copolymer tensio-active agent has a good application prospect.
Claims (10)
1. an AOS-AA copolymer tensio-active agent, it is characterized in that: this AOS-AA copolymer tensio-active agent is generated by polyreaction under the effect of initiator ammonium persulfate by monomer alpha-olefin sodium sulfonate and monomeric acrylic, wherein alpha-olefin sodium sulfonate and acrylic acid mol ratio are 1:(1-4), initiator amount is 0.5 ~ 4.5% of monomer total mass, reaction medium is water, and in reaction system, the mass percent concentration of monomer alpha-olefin sodium sulfonate is 10 ~ 15%.
2. a preparation method for AOS-AA copolymer tensio-active agent according to claim 1, it is characterized in that, concrete steps are as follows:
Monomer alpha-olefin sodium sulfonate, monomeric acrylic, initiator ammonium persulfate and water are joined in the isothermal reaction container of 65 ~ 105 DEG C, insulation reaction 2 ~ 7h, leave standstill after reaction terminates, naturally cool to room temperature, then adjust ph to 8 ~ 9, namely obtain AOS-AA copolymer tensio-active agent.
3. the preparation method of AOS-AA copolymer tensio-active agent according to claim 2, it is characterized in that: described monomer alpha-olefin sodium sulfonate and monomeric acrylic feed intake at twice, the monomer alpha-olefin sodium sulfonate of each input half and the monomeric acrylic of half, the interval time fed intake for twice is 50 ~ 60min.
4. the preparation method of AOS-AA copolymer tensio-active agent according to claim 3, it is characterized in that: described initiator ammonium persulfate takes the mode dripped to feed intake, start to drip initiator continuously when first time drops into monomer alpha-olefin sodium sulfonate and monomeric acrylic, the dropping used time of initiator is 80 ~ 90min, carries out insulation reaction again after dripping initiator.
5. the preparation method of AOS-AA copolymer tensio-active agent according to claim 4, is characterized in that: stir reaction system with the speed of 25 ~ 30r/min in the process dripping initiator.
6. the preparation method of AOS-AA copolymer tensio-active agent according to claim 2, is characterized in that: the speed with 50 ~ 60r/min in insulation reaction process stirs reaction system.
7. the preparation method of AOS-AA copolymer tensio-active agent according to claim 2, is characterized in that: described monomer alpha-olefin sodium sulfonate first filters before use and removes impurity, then regulates its pH value to neutral.
8. the preparation method of AOS-AA copolymer tensio-active agent according to claim 7, is characterized in that: be the NaOH solution adjust ph of 15 ~ 25% with massfraction.
9. AOS-AA copolymer tensio-active agent according to claim 1 is as the application of deinking agent in deinking.
10. the application in deinking agent prepared by AOS-AA copolymer tensio-active agent according to claim 1.
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