CN101781811A - Method for preparing continuous polymerization directly-spun cation-dyeable high-shrinkage polyester staple fibers - Google Patents
Method for preparing continuous polymerization directly-spun cation-dyeable high-shrinkage polyester staple fibers Download PDFInfo
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Abstract
The invention discloses a method for preparing continuous polymerization directly-spun cation-dyeable high-shrinkage polyester staple fibers. A continuous polyester preparation process is adopted, and comprises a process for preparing continuous polymerization modified copolyester melt and a process for preparing directly-spun cation-dyeable high-shrinkage polyester staple fibers; in the process for preparing the continuous polymerization modified copolyester melt, purified terephthalic acid, isophthalic acid, glycol and sodium ethylene glycol isophthalate-5-sulfonate monomers are taken as raw materials to prepare the modified copolyester melt; and then the modified copolyester melt is metered, extruded, blown to be cooled, subjected to oil finish and strand integration, drawn, heat-shaped, coiled and cut to prepare the cation-dyeable high-shrinkage polyester staple fibers. The method has the advantages of short flow, less working procedures, reasonable process, stable melt quality, and good spinning performance; and the prepared high-shrinkage polyester staple fibers have the advantages of good shrinkage stability and even dyeing, and can be dyed by a cation dye, so the production cost is obviously reduced.
Description
Technical field
The present invention relates to a kind of manufacture method of modified copolyester staple fibre, particularly a kind of preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers belongs to the chemical fibre field.
Background technology
Because the numerous premium properties of polyester (terylene) fiber, therefore, it has worldwide obtained development rapidly.But the tight packing of polyester molecule chain, the degree of crystallinity and the degree of orientation are higher, polarity is less, between the polyester long-chain molecule, there is not suitably to hold the gap of dye molecule, therefore dye particles is difficult for entering fiber, its dyeability is poor, can use the kind of dyestuff few, and general polyester fiber can only adopt the dyeing of DISPERSE DYES higher temperature carrier.The cationic dye capable of dyeing modified polyester fiber, owing to have characteristics such as the look of suction is good, beautiful in colour, chromatogram is complete, become the modification kind of present polyesters maximum, and along with continually developing of the continuous expansion of its Application Areas, fabric new product, increasing than the demand of the cation-dyeable high-shrinkage polyester fiber of high shrinkage to having, application prospect is good.
High-shrinkage fibre is meant that fiber boiling water is greater than 25% chemical fibre.According to the difference of its thermal contraction degree, can obtain the final products of different-style and performance.As high-shrinkage polyester staple fibre and other fiber blends, can increase third dimension, bulkiness of fabric etc., on products such as clothes, woollen blanket, Fake Furs, dermatine, be widely used.The cation-dyeable high-shrinkage polyester fiber can also adopt cation dyes to dye except that the performance characteristics with above-mentioned high-shrinkage polyester staple fibre.
The preparation of terylene high-shrinkage fibre mainly contains physical modification or chemical modification and the physical modification two kinds of methods that combine.Physical modification is mainly realized to change the spinning draw conditions, but this its stable contraction rate of high-shrinkage fibre that only makes by physical modification is relatively poor, fibre strength is low, so many at present methods that combine with chemical modification and physical modification are produced, promptly in the production process of normal polyester, pass through to add the 3rd, the 4th monomer, destroy macromolecular regularity, reduce crystallizing power, and in conjunction with the physical modification of spinning drafting process, make the high-shrinkage fibre that makes, boiling water shrinkage height and stable contraction rate, the strength and elongation index is good, satisfies the requirement of back processing better.As Japan Patent (spy opens flat 10-204721), Japan Patent (spy opens flat 10-25620), all disclosed is a kind of " highly shrinkable polyester staple fiber and manufacture method ", it is to adopt the copolyester section that adds M-phthalic acid and other copolymerization component, produces the highly shrinkable polyester staple fiber in conjunction with the change of processing conditions after the spinning.But this series products can only adopt DISPERSE DYES to dye.In order to realize cationic dye capable of dyeing, Japan Patent (spy opens clear 52-3782) discloses a kind of " highly shrinkable copolyester fiber and manufacture method ", it is to adopt the copolyester section that adds ethylene isophthalate-5-sodium sulfonate and other copolymerization component, melt spinning, drawing-off make the highly shrinkable copolyester flock then, and product can adopt cationic dyeing.Publication number CN101173376 is disclosed to be a kind of " manufacture method of cation high shrinkage short fiber ", at first in polyester is synthetic, add the 3rd, the 4th monomer M-phthalic acid and ethylene isophthalate-5-sodium sulfonate, make modified copolyester section, then through the process adjustments production CATION high-shrinkage polyester staple fibers of chip drying, spinning, drawing-off process.
Above-mentioned preparation method is earlier to make the modified copolyester section by chemical modification on the discontinuous polycondensation device, and then modified copolyester is cut into slices crystallization again, drying, fusion are through the physical modification production high-shrinkage fiber of spinning, back processing.The modified copolyester section of on the batchwise polymerization device, producing, exist same batch of material because the discharging time difference, the fluctuation of indexs such as viscosity is bigger, and between criticizing and criticizing, because the cracking of the residual melt of reactor inwall etc., easily cause the difference of properties of product between criticizing and criticizing, these problems all can directly influence the inherent quality of back processing spinning properties and final products.Modified copolyester section simultaneously needs crystallizing and drying and fusion again, and technological process is long, production link is many, production cost is higher.
" polyester industrial " 2003 the 6th phase kings build the article that medium people has delivered a piece " continuous condensed direct-spinning cation dye can dye the exploitation of polyester staple fiber ", its method is on the 50T/D continuous condensed direct spins, and prepares the The cation-dyeable polyester staple fibre by add the 3rd, the 4th monomer ethylene isophthalate-5-sodium sulfonate and adipic acid in Esterification Stage.Low, the steady quality of development product production cost, but this product of researching and producing is meant conventional The cation-dyeable polyester staple fibre.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind of preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers.Technological process of the present invention is short, operation is few, technology is reasonable, and melt quality is stable, good spinning performance; The high-shrinkage polyester staple fibers stable contraction rate that makes is good, even dyeing, and can adopt cationic dyeing, production cost obviously descends.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
A kind of preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers, adopt continuity method polyester manufacture technology, comprise the preparation technology of continuous polymerization modified copolyester melt and the preparation technology of directly-spun cation-dyeable high-shrinkage polyester staple fibre; And adopting p-phthalic acid (PTA), M-phthalic acid (IPA), ethylene glycol (EG) and ethylene isophthalate-5-sodium sulfonate (SIPE) monomer in the preparation technology of continuous polymerization modified copolyester melt is raw material, make the modified copolyester melt, then through measure, extrude, dry cooling, the boundling that oils, drawing-off, HEAT SETTING, curl, cut off technology and make cation-dyeable high-shrinkage polyester staple fibers.
The preparation technology of described modified copolyester melt comprises the steps: at first on continuous polycondensation equipment, adopt p-phthalic acid (PTA), M-phthalic acid (IPA), ethylene glycol (EG) and ethylene isophthalate-5-sodium sulfonate (SIPE) monomer, (IPA) accounts for total dicarboxylic acid (p-phthalic acid by M-phthalic acid, the summation of M-phthalic acid and ethylene isophthalate-5-sodium sulfonate) molar percentage 6.0-10.0, the mol ratio 1 of total dicarboxylic acid and dihydroxylic alcohols (ethylene glycol): 1.15-1: 1.20 ratio is earlier with p-phthalic acid (PTA), M-phthalic acid (IPA), ethylene glycol (EG) measures continuously and stably separately and joins in the slurry still and pulls an oar, and adds catalyst in the making beating still; Above-mentioned slurry continous-stable is delivered in esterification-I, the esterification-II reactor then, add ethylene isophthalate-5-sodium sulfonate (SIPE) and a certain amount of ether of the molar percentage 2.0-4.0 that accounts for total dicarboxylic acid in esterification-II reactor simultaneously continuously and prevent agent, stabilizing agent, 245-255 ℃ of control esterification-II temperature of reaction kettle, time of staying 30-50 minute, the carboxylate that mixes is pumped into polycondensation workshop section, polycondensating process makes the modified copolyester melt at temperature 260-285 ℃ under the condition of vacuum 0.1-10KPa routinely.
The preparation technology of described cation-dyeable high-shrinkage polyester staple fibers comprises the steps: above-mentioned modified copolyester melt, by melt Conveying pipeline equipment, be transported on the corresponding fused mass directly spinning short fiber production equipment, through measure, extrude, dry cooling, boundling oils, drawing-off, HEAT SETTING, curling, cut-out technology, wherein melt Conveying pipeline equipment is by booster pump pressurization, fondant filter filtration, aerial cooler temperature adjustment, and the temperature of control melt Conveying pipeline is 265-275 ℃; Spinning body temperature is 275-285 ℃, spinnerets hole count 2210 or 1560, ring blowing blast 350-400Pa, spinning speed 800-1200 rice/minute, drafting multiple 3.0-4.0,60-90 ℃ of drawing and heat-setting temperature makes boiling water shrinkage greater than 45% cation-dyeable high-shrinkage polyester staple fibers.
Described catalyst adopts a kind of in antimony glycol, antimonous oxide and the antimony acetate.
The anti-agent of described ether can be adopts a kind of in sodium acetate, the potassium acetate.
Described stabilizing agent adopts a kind of in phosphorous acid, trimethyl phosphate and the triphenyl phosphite.
Screw consecutive weighings conveying equipment is adopted in the conveying of described M-phthalic acid powder.
The invention has the beneficial effects as follows: preparation method of the present invention, integrated cost and performance factor, preferred M-phthalic acid (IPA) is as the 3rd monomer, ethylene isophthalate-5-sodium sulfonate (SIPE) is the 4th monomer, in the continuity method polyester manufacture process of routine, by add the IPA of 6.0-10.0% in the slurry preparation process, the SIPE (crowd refers to account for the molar percentage of total dicarboxylic acid) at Esterification Stage interpolation 2.0-4.0% makes the modified copolyester melt; Above-mentioned modified copolyester melt is directly by melt Conveying equipment (pipeline), through measure, extrude, dry cooling, the boundling that oils, drawing-off, HEAT SETTING, curling, cut-out make cationic-dyeable high-shrinkage polyester staple fibre.The preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers of the present invention, because flow process is short, operation is few, technology is reasonable, the content of carboxyl end group of melt (COOH)≤30.0mol/t, inherent viscosity [η] deviation ± 0.010, constant product quality, the fiber boiling water shrinkage that makes is greater than 45%, and stable contraction rate, even dyeing, good spinning performance, production cost obviously descends.
The specific embodiment
Below by specific embodiment, the invention will be further described.Inherent viscosity deviation dl/g wherein, continuity method refers to the poor of inherent viscosity maximum in 24 hours and minimum of a value; Batch process refers to that the head material is poor with the inherent viscosity of tailing in the same batch of material.The mensuration of boiling water shrinkage is the endless tow of getting before cutting off, and is undertaken by the method for testing of general polyester filament.IPA in following examples, the addition of SIPE all refer to account for the molar percentage of total dicarboxylic acid (PTA, IPA and SIPE summation); The content of catalyst, stabilizing agent all refers to account for the percentage by weight of aggregated capacity.
Embodiment 1
The preparation technology of modified copolyester melt: the production capacity of on continuous polycondensation equipment, setting 6000kg/hr, with PTA, IPA and EG monomer account for total dicarboxylic acid (PTA by IPA, IPA and SIPE summation) molar percentage be 6.0, total dicarboxylic acid (PTA, IPA and SIPE summation) join in the slurry still with the mol ratio of dihydroxylic alcohols (EG) by 1: 1.20, pull an oar simultaneously and add the polycondensation catalyst antimony glycol of 450PPM (percentage by weight of aggregated capacity) in the still, above-mentioned slurry continous-stable is delivered in esterification-I reactor, control esterification-I pressure is 0.12MPa, 258.0 ℃ of temperature, material level 60.0%, esterification-I material is sent in esterification-II reactor, 255 ℃ of control esterifications-II temperature of reaction kettle, material level 60.0%, 50 minutes time of staying, add continuously simultaneously and account for total dicarboxylic acid (PTA, IPA and SIPE summation) the allotment concentration of molar percentage 4.0 be 40.0% SIPE, the ether of 300PPM (accounting for the percentage by weight of aggregated capacity) is prevented the agent sodium acetate, the stabilizing agent trimethyl phosphate of 100PPM (accounting for the percentage by weight of aggregated capacity), be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 2
The method of present embodiment is basic identical with embodiment 1, different is: the addition of IPA is 8.0%, 259.0 ℃ of esterifications-I temperature of reaction kettle, 258 ℃ of esterifications-II temperature of reaction kettle, the addition of SIPE is 3.0%, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 3
The method of present embodiment is basic identical with embodiment 1, different is: the addition of IPA is 10.0%, 260.0 ℃ of esterifications-I temperature of reaction kettle, 260 ℃ of esterifications-II temperature of reaction kettle, the addition of SIPE is 2.0%, be pumped into polycondensation workshop section with prepolymer then, polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 4
The method of present embodiment is basic identical with embodiment 1, different is: the addition of IPA is 8.0%, total dicarboxylic acid and dihydroxylic alcohols join in the slurry still by 1: 1.18 mol ratio, 259.0 ℃ of esterifications-I temperature of reaction kettle, 258 ℃ of esterifications-II temperature of reaction kettle, the addition of SIPE is 3.0%, is pumped into polycondensation workshop section with prepolymer then, and polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 5
The method of present embodiment is basic identical with embodiment 1, different is: the addition of IPA is 8.0%, total dicarboxylic acid and dihydroxylic alcohols join in the slurry still by 1: 1.15 mol ratio, 260.0 ℃ of esterifications-I temperature of reaction kettle, 260 ℃ of esterifications-II temperature of reaction kettle, the addition of SIPE is 3.0%, is pumped into polycondensation workshop section with prepolymer then, and polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Embodiment 6
As described in embodiment 4: the modified copolyester melt that embodiment 4 is made, directly by melt Conveying pipeline equipment, be transported on the corresponding fused mass directly spinning short fiber production equipment, through metering, extrude, the blowing cooling, boundling oils, drawing-off, HEAT SETTING, curl, cut off technology, wherein melt Conveying pipeline equipment pressurizes by booster pump, fondant filter filters, the aerial cooler temperature adjustment, the temperature of control melt Conveying pipeline is 270 ℃, spinning body temperature is 280 ℃, spinnerets hole count 2210, ring blowing blast 370Pa, 1000 meters/minute of spinning speeds make as-spun fibre.With the as-spun fibre boundling, set total draft multiple 3.74, the first and second drawing temperatures and be respectively 60 and 75 ℃ then, making specification is 2.22dtex/51mm, and boiling water shrinkage is 51% high-shrinkage polyester staple fibers.(the results are shown in Table 2)
Embodiment 7
As described in embodiment 4: the modified copolyester melt that embodiment 4 is made, directly by melt Conveying pipeline equipment, be transported on the corresponding fused mass directly spinning short fiber production equipment, through metering, extrude, the blowing cooling, boundling oils, drawing-off, HEAT SETTING, curl, cut off technology, wherein melt Conveying pipeline equipment pressurizes by booster pump, fondant filter filters, the aerial cooler temperature adjustment, the temperature of control melt Conveying pipeline is 270 ℃, spinning body temperature is 280 ℃, spinnerets hole count 2210, ring blowing blast 370Pa, 1000 meters/minute of spinning speeds, make as-spun fibre, different is, with the as-spun fibre boundling, set total draft multiple 3.4, first and second drawing temperatures are respectively 65 and 80 ℃, and making specification is 2.22dtex/51mm, and boiling water shrinkage is 47% high-shrinkage polyester staple fibers.(the results are shown in Table 2)
Embodiment 8
As described in embodiment 4: the modified copolyester melt that embodiment 4 is made, directly by melt Conveying pipeline equipment, be transported on the corresponding fused mass directly spinning short fiber production equipment, through metering, extrude, the blowing cooling, boundling oils, drawing-off, HEAT SETTING, curl, cut off technology, wherein melt Conveying pipeline equipment pressurizes by booster pump, fondant filter filters, the aerial cooler temperature adjustment, the temperature of control melt Conveying pipeline is 270 ℃, spinning body temperature is 285 ℃, spinnerets hole count 1560, ring blowing blast 370Pa, 1000 meters/minute of spinning speeds make as-spun fibre.With the as-spun fibre boundling, set 60 and 70 ℃ respectively of total draft multiple 3.5, the first and second drawing temperatures then, making specification is 1.67dtex/38mm, and boiling water shrinkage is 49% high-shrinkage polyester staple fibers.(the results are shown in Table 2)
Embodiment 9
As described in embodiment 4: the modified copolyester melt that embodiment 4 is made, directly by melt Conveying pipeline equipment, be transported on the corresponding fused mass directly spinning short fiber production equipment, through measure, extrude, dry cooling, boundling oils, drawing-off, HEAT SETTING, curling, cut-out technology, wherein melt Conveying pipeline equipment is by booster pump pressurization, fondant filter filtration, aerial cooler temperature adjustment, and the temperature of control melt Conveying pipeline is 270 ℃; Spinning body temperature is 285 ℃, spinnerets hole count 1560, and ring blowing blast 370Pa, 1000 meters/minute of spinning speeds make as-spun fibre.Different is, with the as-spun fibre boundling, sets total draft multiple 3.3, the first and second drawing temperatures and is respectively 65 and 75, and making specification is 1.67dtex/38mm, and boiling water shrinkage is 46% high-shrinkage polyester staple fibers.(the results are shown in Table 2)
Comparative example 1
On production capacity is criticized for about 3500KG/ intermittence polyester equipment, PTA with 2700KG, the IPA of 300KG, the EG monomer of 1500L joins in the slurry still, the stabilizing agent (trimethyl phosphate) that adds 450ml in the making beating still, 1500g polycondensation catalyst (antimony glycol), after mixing, above-mentioned slurry continous-stable is delivered in esterification-I reactor, 255.0 ℃ of control esterifications-I temperature of reaction kettle, pressure is normal pressure, after treating that the water outlet of esterification water reaches 680L, material in esterification-I reactor is sent in esterification-II reactor, and 40.0% SIPE460L is added concentration and is in 240-250 ℃ of control esterification-II temperature of reaction kettle, control time of staying 40-50 minute, esterification finishes, and delivers to polycondensation workshop section with nitrogen pressure then, and polycondensating process makes modified copolyester routinely.(the results are shown in Table 1)
Comparative example 2
As described in comparative example 1: the modified copolyester that comparative example 1 makes is cut into slices, through crystallizing and drying, section moisture content≤50PPM is done in control, extruder temperature is 265-280 ℃, spinning body temperature is 280 ℃, spinnerets hole count 2210, ring blowing blast 370Pa, 1000 meters/minute of spinning speeds make as-spun fibre.With the as-spun fibre boundling, set total draft multiple 3.7, the first and second drawing temperatures and be respectively 60 and 75 ℃ then, making specification is 2.22dtex/51mm, and boiling water shrinkage is 42% high-shrinkage polyester staple fibers.(the results are shown in Table 2)
Comparative example 3
As described in comparative example 1: the modified copolyester that comparative example 1 makes is cut into slices, through crystallizing and drying, section moisture content≤50PPM is done in control, extruder temperature is 270-285 ℃, spinning body temperature is 285 ℃, spinnerets hole count 1560, lateral blowing blast 370Pa, 1000 meters/minute of spinning speeds make as-spun fibre.With the as-spun fibre boundling, set total draft multiple 3.5, the first and second drawing temperatures and be respectively 60 and 70 ℃ then, making specification is 1.67dtex/38mm, and boiling water shrinkage is 40% high-shrinkage polyester staple fibers.(the results are shown in Table 2)
Table 1
Table 2
Claims (7)
1. the preparation method of a continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers, adopt continuity method polyester manufacture technology, it is characterized in that: comprise the preparation technology of continuous polymerization modified copolyester melt and the preparation technology of directly-spun cation-dyeable high-shrinkage polyester staple fibre; And adopting p-phthalic acid, M-phthalic acid, ethylene glycol and ethylene isophthalate-5-sodium sulfonate monomer in the preparation technology of continuous polymerization modified copolyester melt is raw material, makes the modified copolyester melt; Then through measure, extrude, dry cooling, the boundling that oils, drawing-off, HEAT SETTING, curl, cut off technology and make cation-dyeable high-shrinkage polyester staple fibers.
2. the preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers according to claim 1, it is characterized in that: the preparation technology of described modified copolyester melt comprises the steps: at first on continuous polycondensation equipment, adopt the p-phthalic acid, M-phthalic acid, ethylene glycol and ethylene isophthalate-5-sodium sulfonate monomer, molar percentage 6.0-10.0 by the isophthalic acid comprises total dicarboxylic acid, the mol ratio 1 of total dicarboxylic acid and dihydroxylic alcohols: 1.15-1: 1.20 ratio is earlier with the p-phthalic acid, M-phthalic acid, ethylene glycol measures continuously and stably separately and joins in the slurry still and pulls an oar, and adds catalyst in the making beating still; Above-mentioned slurry continous-stable is delivered in esterification-I, the esterification-II reactor then, add ethylene isophthalate-5-sodium sulfonate and the ether of the molar percentage 2.0-4.0 that accounts for total dicarboxylic acid in esterification-II reactor simultaneously continuously and prevent agent, stabilizing agent, 245-255 ℃ of control esterification-II temperature of reaction kettle, time of staying 30-50 minute, the carboxylate that mixes is pumped into polycondensation workshop section, polycondensating process makes the modified copolyester melt at temperature 260-285 ℃ under the condition of vacuum 0.1-10KPa routinely.
3. the preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers according to claim 1, it is characterized in that: the preparation technology of described cation-dyeable high-shrinkage polyester staple fibers comprises the steps: above-mentioned modified copolyester melt, by melt Conveying pipeline equipment, be transported on the corresponding fused mass directly spinning short fiber production equipment, through metering, extrude, the blowing cooling, boundling oils, drawing-off, HEAT SETTING, curl, cut off technology, wherein melt Conveying pipeline equipment pressurizes by booster pump, fondant filter filters, the aerial cooler temperature adjustment, the temperature of control melt Conveying pipeline is 265-275 ℃; Spinning body temperature is 275-285 ℃, spinnerets hole count 2210 or 1560, ring blowing blast 350-400Pa, spinning speed 800-1200 rice/minute, drafting multiple 3.0-4.0,60-90 ℃ of drawing and heat-setting temperature makes boiling water shrinkage greater than 45% cation-dyeable high-shrinkage polyester staple fibers.
4. the preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers according to claim 2 is characterized in that: described catalyst adopts a kind of in antimony glycol, antimonous oxide and the antimony acetate.
5. the preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers according to claim 2 is characterized in that: the anti-agent of described ether can be adopts a kind of in sodium acetate, the potassium acetate.
6. the preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers according to claim 2 is characterized in that: described stabilizing agent adopts a kind of in phosphorous acid, trimethyl phosphate and the triphenyl phosphite.
7. the preparation method of continuous polymerization fused mass directly spinning cation-dyeable high-shrinkage polyester staple fibers according to claim 2 is characterized in that: screw consecutive weighings conveying equipment is adopted in the conveying of described M-phthalic acid powder.
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