CN103409838A - Method for increasing solid content of acrylic fiber spinning solution - Google Patents
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Abstract
The invention discloses a method for increasing solid content of acrylic fiber spinning solution, and belongs to the field of preparation and modification of a functional polymer. 2,2-azodiisobutyronitrile (AIBN) is taken as an initiator; a functional monomer: methacrylic acid-3-sulfydryl propionyloxy ethyl (MMPOE) containing polymerizable double bonds and chain transfer sulfydryl is taken as a branching monomer; branching polyacrylonitrile is compounded under the condition of conventional free radical polymerization; according to certain weight ratio, the compounded branching polyacrylonitrile is mixed with linetype polyacrylonitrile in the NaSCN aqueous solution with a concentration of 58% to obtain the modified acrylic fiber spinning solution. According to the invention, the branching polyacrylonitrile is introduced to the conventional acrylic fiber spinning solution to modify the acrylic fiber spinning solution, so that the viscosity of the acrylic fiber spinning solution is reduced, and the method is simple and practical to operate.
Description
Technical field
The invention belongs to the technical field of branched polymer to the linear polymer modification, relate to a kind of method that improves the liquid-solid body burden of acrylic spinning, by in conventional acrylic spinning liquid, introducing branched polyacrylonitrile, in the situation that do not increase the viscosity of acrylic spinning liquid and do not change its rheological property, can improve the solids content of spinning solution.
Background technology
On polyacrylonitrile (PAN) side chain, with the cyano group of strong polarity, intermolecular force is stronger, makes PAN have rigidity and oil resistivity preferably, is a kind of important polymer, can obtain acrylic fibers by spinning.Acrylic fiber is a kind of important synthetic fiber of Sinopec, has bulkiness, elasticity, warmth retention property, abrasion resistance preferably, is a kind of desirable synthetic fiber that replace wool.In recent years, China's polyacrylonitrile fibre demand is always very large, and higher to the dependence of import acrylic fiber.As 41.7 ten thousand tons of domestic polyacrylonitrile fibre output in 1998, import volume is 37.9 ten thousand tons, and polyacrylonitrile fibre output was 62.9 ten thousand tons in 2003, and import volume is 45.8 ten thousand tons.Current China polyacrylonitrile fibre output is probably at 800,000 tons, but import volume still remains on more than 300,000 tons.Therefore, how to accelerate spinning speed, enhance productivity, reduce costs and become the key issue that the polyacrylonitrile fibre industry is paid close attention to.
Because thermal decomposition at high temperature easily occurs polyacrylonitrile, therefore can not carry out melt spinning, polyacrylonitrile can only be dissolved in solvent and carry out the solution spinning.No matter be, adopt polymerization stoste spinning or at first being settled out polymer prepares spinning solution again, the solids content of spinning solution and viscosity are all important indicators, it is directly connected to the consumption of solvent and speed, energy consumption and the solvent recovery cost of spinning, that is to say directly production cost is played to decisive role, the viscosity of some acrylic fiber spinning solution itself is just very high, so must carry out the viscosity adjusting.Usually, in conventional acrylic fiber spinning solution, the viscosity of polymer itself is very high, if want to reduce the consumption of solvent in spinning process, improve the speed of spinning, attempt to realize by the solids content that improves spinning solution, possible hardly, because the solids content of the every raising 1% of conventional acrylic fiber spinning solution, the viscosity of its spinning solution increases by 35～40%.
Branched polymer is due to the three-dimensional chondritic of its uniqueness, the characteristics such as intermolecular difficult generation chain entanglement, and than linear polymer, it has lower melting viscosity and solution viscosity, hole and good solubility property in a large amount of molecules.Therefore prepare branched polyacrylonitrile, be introduced in conventional acrylic spinning liquid, can effectively reduce the viscosity of spinning solution, thereby improve its solids content, reduce the consumption of solvent, reduce the solvent recovery cost and improve the impact on environment, realizing the low energy consumption of acrylic fiber, the low pollution and highly-efficient processing.
Summary of the invention
The invention discloses a kind of method that improves the liquid-solid body burden of acrylic spinning.It is characterized in that: branched polyacrylonitrile is incorporated in conventional acrylic spinning liquid, it is carried out to modification, can reduce the viscosity of acrylic spinning liquid, operation is simple.In the situation that do not change viscosity and the rheological property of acrylic spinning liquid, can improve the solids content of acrylic spinning liquid, reduce the consumption of solvent, reduce the pollution that solvent recovery cost and production process are brought environment.
A kind of method that improves the liquid-solid body burden of acrylic spinning, according to following step, carry out:
(1) take azodiisobutyronitrile (AIBN) is initator, take and contain the function monomer methacrylic acid that polymerizable double bond and chain shift sulfydryl-3-sulfydryl propionyloxy ethyl ester (MMPOE) and be branched monomer, polymeric reaction temperature is controlled at 60 ℃, with N, N '-dimethyl formamide (DMF) or mass concentration are that 45% sodium sulfocyanate (NaSCN) aqueous solution is under the conventional radical polymerization condition of solvent, synthesizing branched polyacrylonitrile;
(2) branched polyacrylonitrile is incorporated in conventional acrylic spinning liquid, preparation process is: branched polyacrylonitrile and linear polypropylene nitrile are according to the blend in the NaSCN aqueous solution of certain weight ratio, stirring makes polymer dispersed in solution, after dispersed, being placed in 50～70 ℃ of baking ovens dissolves 10～20h and obtains faint yellow transparent acrylic spinning solution, solution left standstill 12～24h in 30～40 ℃ of baking ovens is removed to bubble, obtain the modified acrylic fibers spinning solution.
Wherein the mol ratio of the described azodiisobutyronitrile of step (1) and methacrylic acid-3-sulfydryl propionyloxy ethyl ester is 1.2～2:1.
Wherein the described branched monomer of step (1) accounts for solvent N, 20% of N '-dimethyl formamide gross mass, and branched monomer accounts for 12% of solvent sodium thiocyanate water solution gross mass.
Wherein the mass concentration of the described NaSCN aqueous solution of step (2) is 58%.
Advantage of the present invention: in industrial processes, do not need to change original production technology, branched polyacrylonitrile is incorporated in conventional acrylic spinning liquid, by simple blend, can effectively reduce the viscosity of acrylic spinning liquid, operation is simple.In the situation that do not change viscosity and the rheological property of acrylic spinning liquid, can improve the solids content of acrylic spinning liquid, reduce the consumption of solvent, reduce the pollution that solvent recovery cost and production process are brought environment.Can also reduce simultaneously and filter the diatomaceous consumption of adsorption aid, extend the life-span of spinnerets.
The accompanying drawing explanation:
Fig. 1 be the viscosity of the conventional acrylic spinning liquid of different solids content in embodiment 1 with shear rate change figure,
Fig. 2 be the viscosity of different solids content modified acrylic fibers spinning solution in embodiment 2 with shear rate change figure,
Fig. 3 be the viscosity of 15.7% solids content acrylic spinning liquid with shear rate change figure,
Fig. 4 is the viscosity comparison diagram of embodiment 8 modified acrylic fibers spinning solutions and the conventional acrylic spinning liquid of embodiment 1.
Specific implementation method
Branched polyacrylonitrile described in the present invention, its preparation method (apply for a patent separately, wherein application number: 201110311048.0, denomination of invention: a kind of method for preparing branched polyacrylonitrile) as follows:
Branched polyacrylonitrile preparation method one:
(1) by acrylonitrile (AN, 5mL, 0.076mol), vinylacetate (VAc, 0.8174g, 0.0095mol), MMPOE(0.3767g, 1.73mmol), azodiisobutyronitrile (AIBN, 0.1419g, 0.86mmol) joins and fills concentration is 45% the NaSCN aqueous solution (38.3101g, m
Monomer/ m
Solution=12%), in reaction bulb, after vacuumizing deoxygenation, react 24h under 60 ℃, obtain yellow solution, product is 45% NaSCN aqueous solution dilution through concentration, and dilution is splashed in deionized water and precipitates, the suction filtration drying, obtain faint yellow branched polyacrylonitrile BPAN-1.Adopt three detection gel permeation chromatographs to analyze BPAN-1, result is as follows: absolute weight average molecular weight M
W.MALLS=96800, PDI=2.86, branching factor g'=0.71.
Branched polyacrylonitrile preparation method two:
(2) by acrylonitrile (AN, 5mL, 0.076mol), vinylacetate (VAc, 0.8180g, 0.0095mol), MMPOE(0.2260g, 1.04mmol), AIBN(0.1423g, 0.86mmol) join and fill DMF(20.2936g, m
Monomer/ m
Solution=20%) in the reaction bulb of solution, after vacuumizing deoxygenation, react 48h under 60 ℃, obtain deep yellow solution, product dilutes through DMF, and dilution is splashed in ethanol and precipitates, and the suction filtration drying, obtain faint yellow branched polyacrylonitrile BPAN-2.Adopt three detection gel permeation chromatographs to analyze BPAN-2, result is as follows: absolute weight average molecular weight M
W.MALLS=27160, PDI=2.03, branching factor g'=0.82.
Branched polyacrylonitrile preparation method three:
(3) by acrylonitrile (AN, 5mL, 0.076mol), vinylacetate (VAc, 0.8170g, 0.0095mol), MMPOE(0.3772g, 1.73mmol), AIBN(0.1413g, 0.86mmol), 3-mercaptopropionic acid (0.0458g, 0.43mmol) join that to fill concentration be 45% NaSCN(38.3114g, m
Monomer/ m
Solution=12%), in the reaction bulb of the aqueous solution, after vacuumizing deoxygenation, react 24h under 60 ℃, obtain yellow solution, product is 45% NaSCN aqueous solution dilution through concentration, and dilution is splashed in deionized water and precipitates, the suction filtration drying, obtain faint yellow branched polyacrylonitrile BPAN-3.Adopt three detection gel permeation chromatographs to analyze BPAN-3, result is as follows: absolute weight average molecular weight M
W.MALLS=72410, PDI=2.78, branching factor g'=0.68.
Branched polyacrylonitrile preparation method four:
(4) by acrylonitrile (AN, 5mL, 0.076mol), vinylacetate (VAc, 0.8178g, 0.0095mol), MMPOE(0.3776g, 1.73mmol), AIBN(0.1421g, 0.86mmol), 3-mercaptopropionic acid (0.0916g, 0.86mmol) joins and fills DMF(20.8964g, m
Monomer/ m
Solution=20%) in the reaction bulb of solution, after vacuumizing deoxygenation, react 48h under 60 ℃, obtain deep yellow solution, product dilutes through DMF, and dilution is splashed in ethanol and precipitates, and the suction filtration drying, obtain faint yellow branched polyacrylonitrile BPAN-4.Adopt three detection gel permeation chromatographs to analyze BPAN-4, result is as follows: absolute weight average molecular weight M
W.MALLS=13600, PDI=1.79, branching factor g'=0.70.
By conventional acrylic spinning liquid linear polypropylene nitrile (LPAN, M
W.MALLS=96600,3.0012g) to join concentration be 58% the NaSCN aqueous solution (18.9008g, solids content 13.7%) in, stirring makes dispersed being placed in 60 ℃ of baking ovens of polymer dissolve 10h, obtain yellow solution, again by the 12h deaeration in 30 ℃ of baking ovens of this solution left standstill, obtain solids content and be 13.7% conventional acrylic spinning liquid.Adopt rotational rheometer, in 25 ℃ of rheological curves that record conventional acrylic spinning liquid, as shown in Figure 1, zero shear viscosity is 14.30Pas.
By conventional acrylic spinning liquid linear polypropylene nitrile (LPAN, M
W.MALLS=96600,3.0009g) to join concentration be 58% the NaSCN aqueous solution (17.4111g, solids content 14.7%) in, stirring makes dispersed being placed in 60 ℃ of baking ovens of polymer dissolve 15h, obtain yellow solution, again by the 15h deaeration in 40 ℃ of baking ovens of this solution left standstill, obtain solids content and be 14.7% conventional acrylic spinning liquid.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 1, zero shear viscosity is 20.00Pas, than solids content, is that the zero shear viscosity of 13.7% conventional acrylic spinning liquid has increased by 40%.
By conventional acrylic spinning liquid linear polypropylene nitrile (LPAN, M
W.MALLS=96600,3.0005g) to join concentration be 58% the NaSCN aqueous solution (16.1106g, solids content 15.7%) in, stirring makes dispersed being placed in 70 ℃ of baking ovens of polymer dissolve 20h, obtain yellow solution, again by the 24h deaeration in 40 ℃ of baking ovens of this solution left standstill, obtain solids content and be 15.7% conventional acrylic spinning liquid.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 1, zero shear viscosity is 27.70Pas, than solids content, is that the zero shear viscosity of 13.7% conventional acrylic spinning liquid has increased by 94%.
By synthetic branched polyacrylonitrile (BPAN-1, the M obtained
W.MALLS=96800, g'=0.71; 2.3801g) to join concentration be 58% the NaSCN aqueous solution (15.0003g, solids content 13.7%) in, stirring makes dispersed being placed in 50 ℃ of baking ovens of polymer dissolve 10h, obtain yellow solution, again by the 12h deaeration in 30 ℃ of baking ovens of this solution left standstill, obtain solids content and be 13.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 2, zero shear viscosity is 2.60Pas, than solids content, is that the zero shear viscosity of 13.7% conventional acrylic spinning liquid has reduced by 82%.
By synthetic branched polyacrylonitrile (BPAN-1, the M obtained
W.MALLS=96800, g'=0.71; 2.5804g) to join concentration be 58% the NaSCN aqueous solution (15.0007g, solids content 14.7%) in, stirring makes dispersed being placed in 50 ℃ of baking ovens of polymer dissolve 10h, obtain yellow solution, again by the 12h deaeration in 30 ℃ of baking ovens of this solution left standstill, obtain solids content and be 14.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 2, zero shear viscosity is 2.99Pas, than solids content, is that the zero shear viscosity of 14.7% conventional acrylic spinning liquid has reduced by 85%.
By synthetic branched polyacrylonitrile (BPAN-1, the M obtained
W.MALLS=96800, g'=0.71; 2.7902g) to join concentration be 58% the NaSCN aqueous solution (15.0012g, solids content 15.7%) in, stirring makes dispersed being placed in 50 ℃ of baking ovens of polymer dissolve 10h, obtain yellow solution, again by the 12h deaeration in 30 ℃ of baking ovens of this solution left standstill, obtain solids content and be 15.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 2, zero shear viscosity is 4.72Pas, than solids content, is that the zero shear viscosity of 15.7% conventional acrylic spinning liquid has reduced by 83%.
Embodiment 3
By branched polyacrylonitrile (BPAN-1, M
W.MALLS=96800, g'=0.71; 0.1401g) and linear polypropylene nitrile (LPAN, M
W.MALLS=96600,2.6590g; m
LPAN/ m
BPAN-1=95/5) joining concentration is 58% the NaSCN aqueous solution (15.0309g, solids content 15.7%) in, stirring makes dispersed being placed in 60 ℃ of baking ovens of polymer dissolve 20h, obtain yellow solution, again by the 24h deaeration in 40 ℃ of baking ovens of this solution left standstill, obtain solids content and be 15.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 3, zero shear viscosity is 22.30Pas, than solids content, is that the zero shear viscosity of 15.7% conventional acrylic spinning liquid has reduced by 19%.
Embodiment 4
By branched polyacrylonitrile (BPAN-2, M
W.MALLS=27160, g'=0.82; 0.1403g) and linear polypropylene nitrile (LPAN, M
W.MALLS=96600,2.6593g; m
LPAN/ m
BPAN-2=95/5) joining concentration is 58% the NaSCN aqueous solution (15.0317g, solids content 15.7%) in, stirring makes dispersed being placed in 60 ℃ of baking ovens of polymer dissolve 20h, obtain yellow solution, again by the 24h deaeration in 40 ℃ of baking ovens of this solution left standstill, obtain solids content and be 15.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 3, zero shear viscosity is 23.90Pas, than solids content, is that the zero shear viscosity of 15.7% conventional acrylic spinning liquid has reduced by 14%.
By branched polyacrylonitrile (BPAN-2, M
W.MALLS=27160, g'=0.82; 0.2806g) and linear polypropylene nitrile (LPAN, M
W.MALLS=96600,2.5204g; m
LPAN/ m
BPAN-2=90/10) joining concentration is 58% the NaSCN aqueous solution (15.0321g, solids content 15.7%) in, stirring makes dispersed being placed in 60 ℃ of baking ovens of polymer dissolve 20h, obtain yellow solution, again by the 20h deaeration in 40 ℃ of baking ovens of this solution left standstill, obtain solids content and be 15.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 3, zero shear viscosity is 21.00Pas, than solids content, is that the zero shear viscosity of 15.7% conventional acrylic spinning liquid has reduced by 24%.
Embodiment 6
By branched polyacrylonitrile (BPAN-3, M
W.MALLS=72410, g'=0.68; 0.2805g) and linear polypropylene nitrile (LPAN, M
W.MALLS=96600,2.5201g; m
LPAN/ m
BPAN-3=90/10) joining concentration is 58% the NaSCN aqueous solution (15.0353g, solids content 15.7%) in, stirring makes dispersed being placed in 60 ℃ of baking ovens of polymer dissolve 20h, obtain yellow solution, again by the 20h deaeration in 40 ℃ of baking ovens of this solution left standstill, obtain solids content and be 15.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 3, zero shear viscosity is 20.60Pas, than solids content, is that the zero shear viscosity of 15.7% conventional acrylic spinning liquid has reduced by 26%.
Embodiment 7
By branched polyacrylonitrile (BPAN-4, M
W.MALLS=13600, g'=0.70; 0.2807g) and linear polypropylene nitrile (LPAN, M
W.MALLS=96600,2.5199g; m
LPAN/ m
BPAN-4=90/10) joining concentration is 58% the NaSCN aqueous solution (15.0307g, solids content 15.7%) in, stirring makes dispersed being placed in 60 ℃ of baking ovens of polymer dissolve 20h, obtain yellow solution, again by the 20h deaeration in 40 ℃ of baking ovens of this solution left standstill, obtain solids content and be 15.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 3, zero shear viscosity is 19.10Pas, than solids content, is that the zero shear viscosity of 15.7% conventional acrylic spinning liquid has reduced by 31%.
By branched polyacrylonitrile (BPAN-4, M
W.MALLS=13600, g'=0.70; 0.5609g) and linear polypropylene nitrile (LPAN, M
W.MALLS=96600,2.2411g; m
LPAN/ m
BPAN-4=80/20) joining concentration is 58% the NaSCN aqueous solution (15.0454g, solids content 15.7%) in, stirring makes dispersed being placed in 60 ℃ of baking ovens of polymer dissolve 20h, obtain yellow solution, again by the 20h deaeration in 40 ℃ of baking ovens of this solution left standstill, obtain solids content and be 15.7% modified acrylic fibers spinning solution.Adopt rotational rheometer, in 25 ℃ of rheological curves that record this acrylic spinning liquid, as shown in Figure 4, zero shear viscosity is 13.60Pas, the zero shear viscosity that than solids content is 15.7% conventional acrylic spinning liquid has reduced by 51%, than solids content, is that the zero shear viscosity of 13.7% conventional acrylic spinning liquid has reduced by 5%.
Claims (4)
1. method that improves the liquid-solid body burden of acrylic spinning is characterized in that carrying out according to following step:
(1) take azodiisobutyronitrile (AIBN) is initator, take and contain the function monomer methacrylic acid that polymerizable double bond and chain shift sulfydryl-3-sulfydryl propionyloxy ethyl ester (MMPOE) and be branched monomer, polymeric reaction temperature is controlled at 60 ℃, with N, N '-dimethyl formamide (DMF) or mass concentration are that 45% sodium thiocyanate water solution is under the conventional radical polymerization condition of solvent, synthesizing branched polyacrylonitrile;
(2) branched polyacrylonitrile is incorporated in conventional acrylic spinning liquid, preparation process is: branched polyacrylonitrile and linear polypropylene nitrile are according to the blend in the NaSCN aqueous solution of certain weight ratio, stirring makes polymer dispersed in solution, after dispersed, being placed in 50 ~ 70 ℃ of baking ovens dissolves 10 ~ 20h and obtains faint yellow transparent acrylic spinning solution, solution left standstill 12 ~ 24h in 30 ~ 40 ℃ of baking ovens is removed to bubble, obtain the modified acrylic fibers spinning solution.
2. a kind of method that improves the liquid-solid body burden of acrylic spinning according to claim 1, is characterized in that wherein the mol ratio of the described azodiisobutyronitrile of step (1) and methacrylic acid-3-sulfydryl propionyloxy ethyl ester is 1.2 ~ 2:1;
A kind of method that improves the liquid-solid body burden of acrylic spinning according to claim 1, is characterized in that the wherein mass ratio 5 ~ 100:0 of the described branched polyacrylonitrile of step (2) and linear polypropylene nitrile ~ 95.
3. a kind of method that improves the liquid-solid body burden of acrylic spinning according to claim 1, it is characterized in that wherein the described branched monomer of step (1) accounts for solvent N, 20% of N '-dimethyl formamide gross mass, branched monomer account for 12% of solvent sodium thiocyanate water solution gross mass.
4. a kind of method that improves the liquid-solid body burden of acrylic spinning according to claim 1, is characterized in that wherein the mass concentration of the described NaSCN aqueous solution of step (2) is 58%.
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| CN104611782A (en) * | 2015-01-23 | 2015-05-13 | 常州大学 | Preparation method of anti-pilling acrylon spinning liquid |
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Effective date of registration: 20211220 Address after: Room 407-2-6, building C, Tian'an Digital City, 588 Changwu South Road, Wujin high tech Industrial Development Zone, Changzhou City, Jiangsu Province 213100 Patentee after: CHANGZHOU XIAOGUO INFORMATION SERVICES Co.,Ltd. Address before: Gehu Lake Road Wujin District 213164 Jiangsu city of Changzhou province No. 1 Patentee before: CHANGZHOU University |
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