CN109914110A - A kind of low temperature spinning sizing agent and preparation method thereof - Google Patents
A kind of low temperature spinning sizing agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of low temperature spinning sizing agents and preparation method thereof, belong to textile fabric Sizing Technology field.Present invention introduces 2- methyl-1s, 3-propanediol, primary hydroxyl is brought at its macromolecular chain both ends into, methyl branch can effectively prevent between polyester chain it is close with it is overlapping, the polyester based sizing made has preferable weatherability, counter-bending and stretch-resistance, flexibility, and stability when starching is improved using its preferable adhesion property.Using, containing the stronger ester bond of more than two polarity, the reactivity of starching is improved in molecule, the hydrophilic and lipophilic group of introducing forms the effect of preferable slurry dispersion and emulsion, improves the spreading wetting of slurry, so that starching rate is accelerated.It is denaturalized that low temperature resistant starch is soluble easily in water at low temperature, the loss of slurry is reduced while improving serous coat mechanical property, to increase starching efficiency.The present invention solve current spinning sizing agent cannot after starching under low temperature, starching elongation at break and resistance to flexibility difference problem.
Description
Technical field
The invention belongs to textile fabric Sizing Technology fields, and in particular to a kind of low temperature spinning sizing agent and preparation method thereof.
Background technique
Now widely used sizing fabric slurry mainly has four classes: converted starch, polyvinyl alcohol, polyester and polypropylene
Acid esters slurry.Modified starch size good film-forming property, it is strong with natural fiber affinity, it is easy to desizing, is the main slurry of sizing fabric
Component；But starch size slashing strength is inadequate, not wear-resisting, and inadequate with polyester fiber affinity.Polyvinyl alcohol pulp serous coat
Strength is big, and flexibility is good, and slurry fluidity is good；But polyvinyl alcohol is difficult to desizing, and since polyvinyl alcohol is difficult to degrade, easily
White ambient is caused to pollute, European Union, which has made laws, to be forbidden to use.The chemical structure of polyester pulp is similar to terylene, thus its with wash fibre
It is strong to tie up affinity, is particularly suitable for containing and washs fiber, and its desizing is easy；But polyester pulp easily drops in neutral and alkaline conditions
Solution, hydrolyzes in mashing off and sizing process, causes sizing intensity to decline, limits the application of polyester pulp.Polyacrylic acid
Ester is now widely used sizing auxiliary slurry component, and product form is polyacrylate emulsion and solid propenoic acid ester.Poly- third
Olefin(e) acid emulsion solid content is only 25%, and transportation cost is high；And the presence of emulsifier often deteriorates its service performance, for example generates
Foam influences itself and the compatibility of other class slurries etc..Solid propenoic acid ester slurry is relatively popular, but solid third on the market
The moisture absorption of olefin(e) acid ester slurry is glued seriously again, and film phonograph strength is inadequate.Therefore, whether polyacrylate emulsion or solid propenoic acid ester,
Polyvinyl alcohol still cannot be substituted completely.
Warp yarn sizing is the key link of Textile Engineering, and the main purpose of sizing is to improve the wearability of yarn, is spun at present
It knits slurry and is broadly divided into starch, polyvinyl alcohol, polyacrylic acid three categories slurry, at home and abroad play an important role.But
There is also some problems at present, such as: polyvinyl alcohol pulp cannot degrade, and cause serious environmental problem, by by
Gradually replacing, viscosity is serious again for traditional polypropylene slurry, it is difficult to cause leasing, and Starch Size viscosity fluctuation is big, gelatinizing
It can be poor.The formula of spinning sizing agent is at present, including main slurry and auxiliary slurry.Current main slurry is in view of starching difficulty and upper
Cost is starched, only is difficult to meet starching requirement with single cheap converted starch, often uses converted starch and acrylic pulp
Based on material, PVA mixing slurry, temperature need to be risen to 95 DEG C or more with auxiliary agent and reacted by major ingredient, finally can just obtain slurry, auxiliary slurry
Main finish, the wax disk(-sc) for playing soft smooth.
Using the method for existing slurry sizing, it must prevent temperature from dropping at 90 DEG C or more in starching using existing slurry
Viscosity after low, which increases, influences sizing quality, many sizing faults such as laitance coating, slime spots is also prevented from, so will maintain always in this way
High temperature, quantity of steam waste it is very much, and be continued for high temperature and cannot accomplish production energy-saving, in starching due to sizing machine
In stock tank, there is steam heating and thermal insulation always, the condensed water in steam can be made to be brought into stock tank, reduces the solid content of slurries, cause
The starching amount of sizing changes, and especially the condensed water in cold winter, steam pipe is easy to produce, and is very unstable
, this is also many factories, this is also the key for occurring the partially light problem of starching in sizing process unconsciously.Therefore, how to grind
Sending out a kind of starching at a lower temperature and can guarantee that the stable spinning sizing agent of the yarn property after starching has become and urgently solve at present
Certainly the problem of.
Summary of the invention
The technical problems to be solved by the invention: cannot break after starching in starching under low temperature for current spinning sizing agent
The problem for splitting elongation and resistance to flexibility difference provides a kind of low temperature spinning sizing agent and preparation method thereof.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of low temperature spinning sizing agent, including starching additive, self-emulsifying stabilizer, smooth additive, low temperature resistant binder；
The starching additive the preparation method comprises the following steps: taking alcohol additive 2 ~ 5:2 in mass ratio ~ 6:1 ~ 3 that ester activating agent, 2- first is added
Base -1,3-PD, obtains mixture, is passed through nitrogen protection, and the catalytic additive that mixture quality 1 ~ 3% is added is stirred, then
210 ~ 220 DEG C of heat preservations are warming up to, holding is vacuumized, is cooled to room temperature, filters, takes filtrate up to starching additive.
The alcohol additive are as follows: ethylene glycol, diethylene glycol (DEG), polyethylene glycol-400, polyethylene glycol-4000, neopentyl glycol, 1 are taken,
Any one in 4- butanediol, isobide or it is any it is several by any mass ratio mix to get.
The ester activating agent are as follows: take dimethyl terephthalate (DMT) 5 ~ 10:1 in mass ratio ~ 3 that isophthalic dimethyl ester -5- sulphur is added
The mixing of sour sodium to get.
The catalytic additive mixes the preparation method comprises the following steps: taking glycolic 3 ~ 5:10 in mass ratio ~ 20 that stirring solvent is added,
Mixed liquor is obtained, takes butyl titanate 1 ~ 5:10 ~ 15 to be in mass ratio added dropwise in mixed liquor and is stirred, be cooled to room temperature, is filtered,
Take suction filtration slag washed, it is dry to get catalytic additive.
The solvent are as follows: take tetrahydrofuran 2 ~ 8:2 in mass ratio ~ 5 be added dehydrated alcohol mixing to get.
The self-emulsifying stabilizer the preparation method comprises the following steps:
(1) it takes acid anhydride Activator 2 ~ 5:10 in mass ratio ~ 20 that ethyl acetate is added to be stirred, is cooled to 0 ~ 4 DEG C, obtains cooling
Object takes cooled material 20 ~ 30:2 in mass ratio ~ 5 that cyclopentadiene is added, and vibrates, and filters, and takes and filters slag 3 ~ 7:10 ~ 20 in mass ratio
Petroleum ether and stirring mixing is added, filtering takes filter cake to be evaporated under reduced pressure, and it is dry, obtain dried object；
(2) according to the mass fraction, 40 ~ 50 parts of dried objects, 5 ~ 10 parts of epoxychloropropane, 60 ~ 100 parts of deionized waters, 1 ~ 3 part four are taken
Butylammonium bromide is stirred, and obtains mixture a, takes mixture a 2 ~ 7:10 in mass ratio ~ 20:3 ~ 9 that acetone, methylene chloride is added
It is stirred, obtains mixture b, the sodium hydroxide solution mixing for taking mixture b 10 ~ 30:5 in mass ratio ~ 7 to be added stands, removes
Layer liquid vacuum distillation is to get self-emulsifying stabilizer.
Acid anhydride Activator in the step (1) are as follows: take maleic anhydride 3 ~ 8:2 in mass ratio ~ 5 that 2- phenyl penta is added
Dicarboxylic anhydride mixing to get.
The smooth additive the preparation method comprises the following steps: taking polyoxyethylene 4 ~ 9:1 in mass ratio ~ 4:20 ~ 30 that stearoyl is added
Chlorine, methylene chloride, are passed through nitrogen protection, are stirred, and obtain stirring mixture, take stirring mixture 20 ~ 30:1 ~ 3 in mass ratio
Triethylamine is added to be stirred, mixture a must be stirred, takes stirring mixture a 2 ~ 5:5 in mass ratio ~ 10:30 ~ 50 that water, chlorine is added
Imitative, extraction takes subnatant to be evaporated under reduced pressure to get smooth additive.
The low temperature resistant binder are as follows: hydroxypropyl PASELLI EASYGEL, Ultra Tex 2, acetate is taken to form sediment
Powder, oxidized starch, the double starch adipate of acetylation, hydroxypropul starch, any one in phosphorylation PASELLI EASYGEL are appointed
The mixing of several peaces of anticipating any mass ratioes to get.
The preparation method includes the following steps: that being derived from emulsion stabilizer 2 ~ 5:1 in mass ratio ~ 3 is added Polyethylene glycol-2000
It is stirred, the triphenylphosphine of self-emulsifying stabilizer quality 1 ~ 4% is added, kept the temperature in 120 ~ 130 DEG C, be cooled to room temperature, obtain cooling
Object a takes 200 ~ 250 parts of starching additives, 10 ~ 15 parts of cooled material a, 20 ~ 30 parts of smooth additives, 30 ~ 50 according to the mass fraction
The low temperature resistant binder of part, 100 ~ 150 parts of water are stirred to get low temperature spinning sizing agent.
The present invention is compared with other methods, and advantageous effects are:
(1) starching additive prepared by the present invention is to be added in the process with alcohol additive and ester activating agent through catalytic esterification
Glycolic and butyl titanate obtain the cricoid catalytic activity agent of oil base, and major cyclic chelating effect improves its resistant to hydrolysis energy
Power introduces 2- methyl-1,3-propanediol so that the efficiency of catalyzed conversion improves, and primary hydroxyl is brought at macromolecular chain both ends into, benefit
Shorten the time that the reaction participated in carries out with high reaction activity, and introduce methyl branch can effectively prevent between polyester chain
It is close with it is overlapping so that the obtained preferable weatherability of polyester based sizing, counter-bending and stretch-resistance, flexibility, using its compared with
Stability when good adhesion property improves starching is good, while polyester will not be congealed into ice at quite low temperatures
Shape, so that keeping starch finishing effect at low temperature；
(2) self-emulsifying stabilizer prepared by the present invention is reacted with acid anhydride Activator, cyclopentadiene, then through epoxychloropropane
The ring-opening reaction that nucleophilic addition occurs obtains, on the one hand using the stronger ester bond of more than two polarity is contained in molecule, with fiber
The intermolecular formation crosslinking of base, is improved the reactivity of starching, is on the other hand formed preferably using the hydrophilic and lipophilic group of introducing
The effect of slurry dispersion and emulsion so that between each component of slurry compatibility improve, and by reduce starching when with fiber contacts circle
The surface tension in face improves the spreading wetting of slurry, so that starching rate is accelerated；
(3) smooth additive prepared by the present invention is to be reacted to obtain with polyoxyethylene, stearyl chloride, stearic acid polyoxyethylene
Ester molecule ethylene oxide is condensed, and the coefficient of friction for reducing serosa surface when slurry sizing is made after addition, improves serous coat
Toughness is allowed to obtain soft and smooth effect, forms gravity flow flat surface in fiber surface, improves the performance of starching, finally plus
Enter low temperature resistant binder, it is soluble easily in water at low temperature with the starch for being denaturalized low temperature resistant, the substance of starching cementing property is formed, in fibre
Surface filming is tieed up, so that each component of starching is adhered to fiber and forms preferable bonding interface, is improving serous coat mechanical property
While reduce slurry loss, to increase starching efficiency.
(4) present invention first passes through starching additive, so that the obtained preferable weatherability of polyester based sizing, counter-bending and anti-
Draftability, flexibility, stability when improving starching using its preferable adhesion property is good, while making polyester very low
At a temperature of will not condense into ice-like so that keeping starch finishing effect at low temperature, using self-emulsifying stabilizer, utilize introducing
Hydrophilic and lipophilic group forms the effect of preferable slurry dispersion and emulsion, surface tension when reducing starching with fiber contacts interface,
The spreading wetting of slurry is improved, starching rate is improved, finally makes to bond film forming in fiber surface using smooth additive, improve
Self-leveling, so that starching surface is smooth.
Specific embodiment
Alcohol additive are as follows: take ethylene glycol, diethylene glycol (DEG), polyethylene glycol-400, polyethylene glycol-4000, neopentyl glycol, 1,4- fourth
Any one in glycol, isobide or it is any it is several by any mass ratio mix to get.
Ester activating agent are as follows: take dimethyl terephthalate (DMT) 5 ~ 10:1 in mass ratio ~ 3 that isophthalic dimethyl ester -5- sodium sulfonate is added
Mixing to get.
Solvent are as follows: take tetrahydrofuran 2 ~ 8:2 in mass ratio ~ 5 be added dehydrated alcohol mixing to get.
Catalytic additive the preparation method comprises the following steps: take glycolic 3 ~ 5:10 in mass ratio ~ 20 be added solvent, be warming up to 50 ~ 60
DEG C it is stirred 20 ~ 30min, obtains mixed liquor, butyl titanate 1 ~ 5:10 ~ 15 in mass ratio is taken to be added dropwise in mixed liquor, heated up
It is stirred 2 ~ 4h to 70 ~ 80 DEG C, is cooled to room temperature, is filtered, takes suction filtration slag to wash through dehydrated alcohol, drying adds to get catalysis
Add agent.
Starching additive the preparation method comprises the following steps: taking alcohol additive 2 ~ 5:2 in mass ratio ~ 6:1 ~ 3 that ester activating agent, 2- first is added
Base -1,3-PD, obtains mixture, is passed through nitrogen protection, and the catalytic additive of mixture quality 1 ~ 3% is added, it is warming up to 170 ~
180 DEG C are stirred 1 ~ 3h, then are warming up to 210 ~ 220 DEG C of 1 ~ 3h of heat preservation, vacuumize 40 ~ 60min of holding, are cooled to room temperature, mistake
Filter, takes filtrate up to starching additive.
Acid anhydride Activator are as follows: take maleic anhydride 3 ~ 8:2 in mass ratio ~ 5 that the mixing of 2- phenyl glutaric anhydride is added, i.e.,
?.
Self-emulsifying stabilizer the preparation method comprises the following steps:
(1) it takes acid anhydride Activator 2 ~ 5:10 in mass ratio ~ 20 that ethyl acetate is added, is stirred 20 ~ 40min in 40 ~ 60 DEG C, it is cold
But to 0 ~ 4 DEG C, cooled material is obtained, takes cooled material 20 ~ 30:2 in mass ratio ~ 5 that cyclopentadiene is added, in 0 ~ 4 DEG C of 30 ~ 60min of oscillation,
It filters, takes and filter slag 3 ~ 7:10 in mass ratio ~ 20 addition petroleum ether, be stirred 30 ~ 90min in 40 ~ 70 DEG C, filter, take filter
Cake vacuum distillation, it is dry, obtain dried object；
(2) according to the mass fraction, 40 ~ 50 parts of dried objects, 5 ~ 10 parts of epoxychloropropane, 60 ~ 100 parts of deionized waters, 1 ~ 3 part four are taken
Butylammonium bromide is warming up to 100 ~ 110 DEG C and is stirred 1 ~ 3h, obtains mixture a, takes mixture a 2 ~ 7:10 in mass ratio ~ 20:3
~ 9 be added acetone, methylene chloride, be stirred 30 ~ 50min in 40 ~ 50 DEG C, obtain mixture b, take mixture b in mass ratio 10 ~
30:5 ~ 7 is added the sodium hydroxide solution that mass fraction is 30% and mixes, and stands, takes subnatant to be evaporated under reduced pressure steady to get self-emulsifying
Determine agent.
Smooth additive the preparation method comprises the following steps: taking polyoxyethylene 4 ~ 9:1 in mass ratio ~ 4:20 ~ 30 that stearyl chloride, two is added
Chloromethanes is passed through nitrogen protection, is stirred 50 ~ 60min in 80 ~ 90 DEG C, obtains stirring mixture, takes stirring mixture by quality
Than 20 ~ 30:1 ~ 3 be added triethylamine, be stirred 60 ~ 90min in 80 ~ 90 DEG C, must stir mixture a, take stir mixture a by
Water, chloroform is added in 2 ~ 5:5 of mass ratio ~ 10:30 ~ 50, and extraction takes subnatant to be evaporated under reduced pressure to get smooth additive.
Low temperature resistant binder are as follows: take hydroxypropyl PASELLI EASYGEL, Ultra Tex 2, acetate starch, oxygen
Change starch, the double starch adipate of acetylation, hydroxypropul starch, any one in phosphorylation PASELLI EASYGEL or any several
By any mass ratio mix to get.
A kind of preparation method of low temperature spinning sizing agent includes the following steps: to be derived from emulsion stabilizer 2 ~ 5:1 ~ 3 in mass ratio
Polyethylene glycol-2000 is added, is warming up to 120 ~ 130 DEG C and is stirred 20 ~ 40min, self-emulsifying stabilizer quality 1 ~ 4% is added
Triphenylphosphine is cooled to room temperature in 120 ~ 130 DEG C of 2 ~ 4h of heat preservation, obtains cooled material a, according to the mass fraction, take on 200 ~ 250 parts
It is mixed to starch additive, 10 ~ 15 parts of cooled material a, 20 ~ 30 parts of smooth additives, 30 ~ 50 parts of low temperature resistant binders, 100 ~ 150 parts of water
It closes, is stirred 1 ~ 3h in 40 ~ 60 DEG C to get low temperature spinning sizing agent.
Embodiment 1
Alcohol additive are as follows: take ethylene glycol, diethylene glycol (DEG) by any mass ratio mix to get.
Ester activating agent are as follows: take dimethyl terephthalate (DMT) 5:1 in mass ratio that the mixing of isophthalic dimethyl ester -5- sodium sulfonate is added,
To obtain the final product.
Solvent are as follows: take tetrahydrofuran 2:2 in mass ratio be added dehydrated alcohol mixing to get.
Catalytic additive the preparation method comprises the following steps: take glycolic 3:10 in mass ratio that solvent is added, it is mixed to be warming up to 50 DEG C of stirrings
20min is closed, mixed liquor is obtained, butyl titanate 1:10 in mass ratio is taken to be added dropwise in mixed liquor, be warming up to 70 DEG C and be stirred 2h,
It is cooled to room temperature, filters, suction filtration slag is taken to wash through dehydrated alcohol, it is dry to get catalytic additive.
Starching additive the preparation method comprises the following steps: take alcohol additive 2:2:1 in mass ratio be added ester activating agent, 2- methyl-1,
3-propanediol obtains mixture, is passed through nitrogen protection, and the catalytic additive of mixture quality 1% is added, and it is mixed to be warming up to 170 DEG C of stirrings
1h is closed, then is warming up to 210 DEG C of heat preservation 1h, vacuumizes and keeps 40min, be cooled to room temperature, is filtered, takes filtrate up to starching addition
Agent.
Acid anhydride Activator are as follows: take maleic anhydride 3:2 in mass ratio be added 2- phenyl glutaric anhydride mixing to get.
Self-emulsifying stabilizer the preparation method comprises the following steps:
(1) it takes acid anhydride Activator 2:10 in mass ratio that ethyl acetate is added, is stirred 20min in 40 DEG C, is cooled to 0 DEG C, obtains
Cooled material takes cooled material 20:2 in mass ratio that cyclopentadiene is added, and in 0 DEG C of oscillation 30min, filters, takes and filter slag in mass ratio
Petroleum ether is added in 3:10, is stirred 30min in 40 DEG C, filters, filter cake is taken to be evaporated under reduced pressure, dry, obtains dried object；
(2) according to the mass fraction, 40 parts of dried objects, 5 parts of epoxychloropropane, 60 parts of deionized waters, 1 part of tetrabutylammonium bromide are taken,
It is warming up to 100 DEG C and is stirred 1h, obtain mixture a, take mixture a 2:10:3 in mass ratio that acetone, methylene chloride is added, in 40
DEG C it is stirred 30min, obtains mixture b, takes mixture b 10:5 in mass ratio that the sodium hydroxide that mass fraction is 30% is added molten
Liquid mixing, stands, takes subnatant to be evaporated under reduced pressure to get self-emulsifying stabilizer.
Smooth additive the preparation method comprises the following steps: take polyoxyethylene 4:1:20 in mass ratio that stearyl chloride, methylene chloride is added,
It is passed through nitrogen protection, 50min is stirred in 80 DEG C, obtains stirring mixture, stirring mixture 20:1 in mass ratio is taken to be added three
Ethamine is stirred 60min in 80 DEG C, must stir mixture a, takes stirring mixture a 2:5:30 in mass ratio that water, chlorine is added
Imitative, extraction takes subnatant to be evaporated under reduced pressure to get smooth additive.
Low temperature resistant binder are as follows: take hydroxypropyl PASELLI EASYGEL, Ultra Tex 2 mixed by any mass ratio
Close to get.
A kind of preparation method of low temperature spinning sizing agent includes the following steps: to be derived from emulsion stabilizer 2:1 in mass ratio addition
Polyethylene glycol-2000 is warming up to 120 DEG C and is stirred 20min, the triphenylphosphine of self-emulsifying stabilizer quality 1% is added, in 120
DEG C heat preservation 2h, be cooled to room temperature, obtain cooled material a, according to the mass fraction, take 200 parts of starching additives, 10 parts of cooled material a, 20 parts
Smooth additive, 30 parts of low temperature resistant binders, 100 parts of water mixing, are stirred 1h in 40 DEG C to get low temperature spinning sizing agent.
Embodiment 2
Alcohol additive are as follows: taking polyethylene glycol -400, polyethylene glycol-4000 by any mass ratio mix to get.
Ester activating agent are as follows: take dimethyl terephthalate (DMT) 8:2 in mass ratio that the mixing of isophthalic dimethyl ester -5- sodium sulfonate is added,
To obtain the final product.
Solvent are as follows: take tetrahydrofuran 5:4 in mass ratio be added dehydrated alcohol mixing to get.
Catalytic additive the preparation method comprises the following steps: take glycolic 4:15 in mass ratio that solvent is added, it is mixed to be warming up to 55 DEG C of stirrings
25min is closed, mixed liquor is obtained, butyl titanate 3:12 in mass ratio is taken to be added dropwise in mixed liquor, be warming up to 75 DEG C and be stirred 3h,
It is cooled to room temperature, filters, suction filtration slag is taken to wash through dehydrated alcohol, it is dry to get catalytic additive.
Starching additive the preparation method comprises the following steps: take alcohol additive 4:4:2 in mass ratio be added ester activating agent, 2- methyl-1,
3-propanediol obtains mixture, is passed through nitrogen protection, and the catalytic additive of mixture quality 2% is added, and it is mixed to be warming up to 175 DEG C of stirrings
2h is closed, then is warming up to 215 DEG C of heat preservation 2h, vacuumizes and keeps 50min, be cooled to room temperature, is filtered, takes filtrate up to starching addition
Agent.
Acid anhydride Activator are as follows: take maleic anhydride 5:3 in mass ratio be added 2- phenyl glutaric anhydride mixing to get.
Self-emulsifying stabilizer the preparation method comprises the following steps:
(1) it takes acid anhydride Activator 3:15 in mass ratio that ethyl acetate is added, is stirred 30min in 50 DEG C, is cooled to 2 DEG C, obtains
Cooled material takes cooled material 25:3 in mass ratio that cyclopentadiene is added, and in 2 DEG C of oscillation 45min, filters, takes and filter slag in mass ratio
Petroleum ether is added in 5:15, is stirred 60min in 55 DEG C, filters, filter cake is taken to be evaporated under reduced pressure, dry, obtains dried object；
(2) according to the mass fraction, 45 parts of dried objects, 8 parts of epoxychloropropane, 80 parts of deionized waters, 2 parts of tetrabutylammonium bromide are taken,
It is warming up to 105 DEG C and is stirred 2h, obtain mixture a, take mixture a 4:15:6 in mass ratio that acetone, methylene chloride is added, in 45
DEG C it is stirred 40min, obtains mixture b, takes mixture b 20:6 in mass ratio that the sodium hydroxide that mass fraction is 30% is added molten
Liquid mixing, stands, takes subnatant to be evaporated under reduced pressure to get self-emulsifying stabilizer.
Smooth additive the preparation method comprises the following steps: take polyoxyethylene 6:3:25 in mass ratio that stearyl chloride, methylene chloride is added,
It is passed through nitrogen protection, 55min is stirred in 85 DEG C, obtains stirring mixture, stirring mixture 25:2 in mass ratio is taken to be added three
Ethamine is stirred 75min in 85 DEG C, must stir mixture a, takes stirring mixture a 4:8:40 in mass ratio that water, chlorine is added
Imitative, extraction takes subnatant to be evaporated under reduced pressure to get smooth additive.
Low temperature resistant binder are as follows: take acetate starch, oxidized starch by any mass ratio mix to get.
A kind of preparation method of low temperature spinning sizing agent includes the following steps: to be derived from emulsion stabilizer 4:2 in mass ratio addition
Polyethylene glycol-2000 is warming up to 125 DEG C and is stirred 30min, the triphenylphosphine of self-emulsifying stabilizer quality 3% is added, in 125
DEG C heat preservation 3h, be cooled to room temperature, obtain cooled material a, according to the mass fraction, take 225 parts of starching additives, 12 parts of cooled material a, 25 parts
Smooth additive, 40 parts of low temperature resistant binders, 125 parts of water mixing, are stirred 2h in 50 DEG C to get low temperature spinning sizing agent.
Embodiment 3
Alcohol additive are as follows: take neopentyl glycol, 1,4-butanediol, isobide by any mass ratio mix to get.
Ester activating agent are as follows: take dimethyl terephthalate (DMT) 10:3 in mass ratio that the mixing of isophthalic dimethyl ester -5- sodium sulfonate is added,
To obtain the final product.
Solvent are as follows: take tetrahydrofuran 8:5 in mass ratio be added dehydrated alcohol mixing to get.
Catalytic additive the preparation method comprises the following steps: take glycolic 5:20 in mass ratio that solvent is added, it is mixed to be warming up to 60 DEG C of stirrings
30min is closed, mixed liquor is obtained, butyl titanate 5:15 in mass ratio is taken to be added dropwise in mixed liquor, be warming up to 80 DEG C and be stirred 4h,
It is cooled to room temperature, filters, suction filtration slag is taken to wash through dehydrated alcohol, it is dry to get catalytic additive.
Starching additive the preparation method comprises the following steps: take alcohol additive 5:6:3 in mass ratio be added ester activating agent, 2- methyl-1,
3-propanediol obtains mixture, is passed through nitrogen protection, and the catalytic additive of mixture quality 3% is added, and it is mixed to be warming up to 180 DEG C of stirrings
3h is closed, then is warming up to 220 DEG C of heat preservation 3h, vacuumizes and keeps 60min, be cooled to room temperature, is filtered, takes filtrate up to starching addition
Agent.
Acid anhydride Activator are as follows: take maleic anhydride 8:5 in mass ratio be added 2- phenyl glutaric anhydride mixing to get.
Self-emulsifying stabilizer the preparation method comprises the following steps:
(1) it takes acid anhydride Activator 5:20 in mass ratio that ethyl acetate is added, is stirred 40min in 60 DEG C, is cooled to 4 DEG C, obtains
Cooled material takes cooled material 30:5 in mass ratio that cyclopentadiene is added, and in 4 DEG C of oscillation 60min, filters, takes and filter slag in mass ratio
Petroleum ether is added in 7:20, is stirred 90min in 70 DEG C, filters, filter cake is taken to be evaporated under reduced pressure, dry, obtains dried object；
(2) according to the mass fraction, 50 parts of dried objects, 10 parts of epoxychloropropane, 100 parts of deionized waters, 3 parts of tetrabutyl phosphonium bromides are taken
Ammonium is warming up to 110 DEG C and is stirred 3h, obtains mixture a, takes mixture a 7:20:9 in mass ratio that acetone, methylene chloride is added,
It is stirred 50min in 50 DEG C, obtains mixture b, takes mixture b 30:7 in mass ratio that the hydroxide that mass fraction is 30% is added
Sodium solution mixing, stands, takes subnatant to be evaporated under reduced pressure to get self-emulsifying stabilizer.
Smooth additive the preparation method comprises the following steps: take polyoxyethylene 9:4:30 in mass ratio that stearyl chloride, methylene chloride is added,
It is passed through nitrogen protection, 60min is stirred in 90 DEG C, obtains stirring mixture, stirring mixture 30:3 in mass ratio is taken to be added three
Ethamine is stirred 90min in 90 DEG C, must stir mixture a, takes stirring mixture a 5:10:50 in mass ratio that water, chlorine is added
Imitative, extraction takes subnatant to be evaporated under reduced pressure to get smooth additive.
Low temperature resistant binder are as follows: take the double starch adipate of acetylation, hydroxypropul starch, phosphorylation PASELLI EASYGEL by
Any mass ratio mixing to get.
A kind of preparation method of low temperature spinning sizing agent includes the following steps: to be derived from emulsion stabilizer 5:3 in mass ratio addition
Polyethylene glycol-2000 is warming up to 130 DEG C and is stirred 40min, the triphenylphosphine of self-emulsifying stabilizer quality 4% is added, in 130
DEG C heat preservation 4h, be cooled to room temperature, obtain cooled material a, according to the mass fraction, take 250 parts of starching additives, 15 parts of cooled material a, 30 parts
Smooth additive, 50 parts of low temperature resistant binders, 150 parts of water mixing, are stirred 3h in 60 DEG C to get low temperature spinning sizing agent.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking starching additive.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking self-emulsifying stabilizer.
Comparative example 3: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking smooth additive.
Comparative example 4: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking low temperature resistant binder.
Comparative example 5: the low temperature spinning sizing agent of company, Wuhu City production.
Embodiment is tested with low temperature spinning sizing agent obtained by comparative example according to FZ/T 15001-2008, test result
It is as shown in table 1:
Table 1:
In summary, the resulting low temperature spinning sizing agent starch finishing effect of the present invention is preferable, has good viscosity thermal stability and glues
Attached power, it is more preferable compared to commercial product effect, it is worth promoting.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of low temperature spinning sizing agent, which is characterized in that including starching additive, self-emulsifying stabilizer, smooth additive, resistance to low
Warm binder；
The starching additive the preparation method comprises the following steps: taking alcohol additive 2 ~ 5:2 in mass ratio ~ 6:1 ~ 3 that ester activating agent, 2- first is added
Base -1,3-PD, obtains mixture, is passed through nitrogen protection, and the catalytic additive that mixture quality 1 ~ 3% is added is stirred, then
210 ~ 220 DEG C of heat preservations are warming up to, holding is vacuumized, is cooled to room temperature, filters, takes filtrate up to starching additive.
2. low temperature spinning sizing agent according to claim 1, which is characterized in that the alcohol additive are as follows: take ethylene glycol, two sweet
Alcohol, polyethylene glycol-400, polyethylene glycol-4000, neopentyl glycol, 1,4- butanediol, any one in isobide or any several
Kind by any mass ratio mix to get.
3. low temperature spinning sizing agent according to claim 1, which is characterized in that the ester activating agent are as follows: take terephthalic acid (TPA)
Dimethyl ester 5 ~ 10:1 in mass ratio ~ 3 be added isophthalic dimethyl ester -5- sodium sulfonate mixing to get.
4. low temperature spinning sizing agent according to claim 1, which is characterized in that the catalytic additive the preparation method comprises the following steps:
It takes glycolic 3 ~ 5:10 in mass ratio ~ 20 that stirring solvent mixing is added, obtains mixed liquor, take butyl titanate 1 ~ 5:10 in mass ratio
~ 15 are added dropwise in mixed liquor and are stirred, and are cooled to room temperature, and filter, and take that filter slag washed, dry to get catalytic additive.
5. low temperature spinning sizing agent according to claim 4, which is characterized in that the solvent are as follows: take tetrahydrofuran by quality
Than 2 ~ 8:2 ~ 5 be added dehydrated alcohol mixing to get.
6. low temperature spinning sizing agent according to claim 1, which is characterized in that the preparation method of the self-emulsifying stabilizer
Are as follows:
(1) it takes acid anhydride Activator 2 ~ 5:10 in mass ratio ~ 20 that ethyl acetate is added to be stirred, is cooled to 0 ~ 4 DEG C, obtains cooling
Object takes cooled material 20 ~ 30:2 in mass ratio ~ 5 that cyclopentadiene is added, and vibrates, and filters, and takes and filters slag 3 ~ 7:10 ~ 20 in mass ratio
Petroleum ether and stirring mixing is added, filtering takes filter cake to be evaporated under reduced pressure, and it is dry, obtain dried object；
(2) according to the mass fraction, 40 ~ 50 parts of dried objects, 5 ~ 10 parts of epoxychloropropane, 60 ~ 100 parts of deionized waters, 1 ~ 3 part four are taken
Butylammonium bromide is stirred, and obtains mixture a, takes mixture a 2 ~ 7:10 in mass ratio ~ 20:3 ~ 9 that acetone, methylene chloride is added
It is stirred, obtains mixture b, the sodium hydroxide solution mixing for taking mixture b 10 ~ 30:5 in mass ratio ~ 7 to be added stands, removes
Layer liquid vacuum distillation is to get self-emulsifying stabilizer.
7. low temperature spinning sizing agent according to claim 6, which is characterized in that the acid anhydride Activator in the step (1) are as follows:
Take maleic anhydride 3 ~ 8:2 in mass ratio ~ 5 be added 2- phenyl glutaric anhydride mixing to get.
8. low temperature spinning sizing agent according to claim 1, which is characterized in that the smooth additive the preparation method comprises the following steps:
It takes polyoxyethylene 4 ~ 9:1 in mass ratio ~ 4:20 ~ 30 that stearyl chloride, methylene chloride is added, is passed through nitrogen protection, is stirred, obtain
Mixture is stirred, takes stirring mixture 20 ~ 30:1 in mass ratio ~ 3 that triethylamine is added and is stirred, mixture a must be stirred, take and stir
It mixes mixture a 2 ~ 5:5 in mass ratio ~ 10:30 ~ 50 and water, chloroform is added, extraction takes subnatant to be evaporated under reduced pressure to get smooth addition
Agent.
9. low temperature spinning sizing agent according to claim 1, which is characterized in that the low temperature resistant binder are as follows: take hydroxypropyl
PASELLI EASYGEL, Ultra Tex 2, acetate starch, oxidized starch, acetylation double starch adipates, hydroxypropyl
Any one in base starch, phosphorylation PASELLI EASYGEL or any mass ratio mixing of any several peaces to get.
10. a kind of preparation method of the low temperature spinning sizing agent as described in claim 1 ~ 9 any one, which is characterized in that the system
Preparation Method includes the following steps: that being derived from emulsion stabilizer 2 ~ 5:1 in mass ratio ~ 3 addition Polyethylene glycol-2000 is stirred, and adds
The triphenylphosphine for entering self-emulsifying stabilizer quality 1 ~ 4% keeps the temperature in 120 ~ 130 DEG C, is cooled to room temperature, cooled material a is obtained, by quality
Number meter, take 200 ~ 250 parts of starching additives, 10 ~ 15 parts of cooled material a, 20 ~ 30 parts of smooth additives, 30 ~ 50 parts it is low temperature resistant viscous
Knot agent, 100 ~ 150 parts of water are stirred to get low temperature spinning sizing agent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114032689A (en) * | 2021-12-15 | 2022-02-11 | 温州百德富新材料有限公司 | Water-based woven tape sizing slurry and preparation method thereof |
| CN114381942A (en) * | 2021-12-20 | 2022-04-22 | 江南大学 | Sizing agent for preventing Lycra cotton yarn from bonding and sizing process thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102182060A (en) * | 2011-03-11 | 2011-09-14 | 徐州众恒淀粉科技有限公司 | Special slurry for sizing warp containing polyester staple fibers |
| CN104151535A (en) * | 2014-08-09 | 2014-11-19 | 河北工业大学 | Segmented polyester copolymer and preparation method thereof |
| CN104370863A (en) * | 2014-11-25 | 2015-02-25 | 南京工业大学 | Preparation method of exo-type nadic anhydride |
| US20170342275A1 (en) * | 2016-05-27 | 2017-11-30 | Daikin Industries, Ltd. | Water-based surface treatment agent |
| CN109267341A (en) * | 2018-08-21 | 2019-01-25 | 中纺院（浙江）技术研究院有限公司 | A kind of slurry and its mixing method and sizing technique |
-
2019
- 2019-02-20 CN CN201910124837.XA patent/CN109914110A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102182060A (en) * | 2011-03-11 | 2011-09-14 | 徐州众恒淀粉科技有限公司 | Special slurry for sizing warp containing polyester staple fibers |
| CN104151535A (en) * | 2014-08-09 | 2014-11-19 | 河北工业大学 | Segmented polyester copolymer and preparation method thereof |
| CN104370863A (en) * | 2014-11-25 | 2015-02-25 | 南京工业大学 | Preparation method of exo-type nadic anhydride |
| US20170342275A1 (en) * | 2016-05-27 | 2017-11-30 | Daikin Industries, Ltd. | Water-based surface treatment agent |
| CN109267341A (en) * | 2018-08-21 | 2019-01-25 | 中纺院（浙江）技术研究院有限公司 | A kind of slurry and its mixing method and sizing technique |
Non-Patent Citations (2)
| Title |
|---|
| N.勋弗尔特: "《非离子表面活性剂的制造、性能和分析》", 30 June 1990, 轻工业出版社 * |
| 刘森主编: "《机织技术》", 30 June 2006, 中国纺织出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114032689A (en) * | 2021-12-15 | 2022-02-11 | 温州百德富新材料有限公司 | Water-based woven tape sizing slurry and preparation method thereof |
| CN114032689B (en) * | 2021-12-15 | 2023-12-26 | 温州百德富新材料有限公司 | Aqueous braid sizing slurry and preparation method thereof |
| CN114381942A (en) * | 2021-12-20 | 2022-04-22 | 江南大学 | Sizing agent for preventing Lycra cotton yarn from bonding and sizing process thereof |
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Application publication date: 20190621 |