CN1182812A - Method for imparting lubricity to synthetic fiber filament yarn subjected to contact heating type false twisting - Google Patents
Method for imparting lubricity to synthetic fiber filament yarn subjected to contact heating type false twisting Download PDFInfo
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- CN1182812A CN1182812A CN 97122873 CN97122873A CN1182812A CN 1182812 A CN1182812 A CN 1182812A CN 97122873 CN97122873 CN 97122873 CN 97122873 A CN97122873 A CN 97122873A CN 1182812 A CN1182812 A CN 1182812A
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- lubricant
- synthetic fiber
- heating type
- false twisting
- contact heating
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Abstract
The invention provides a method for imparting lubricity to synthetic fiber filament yarn for contact heating type false twisting, which can prevent the synthetic fiber filament yarn from being polluted by a heater in the contact heating type false twisting. An aqueous liquid of a lubricant or a treating agent containing a lubricant having a specific composition is adjusted to a predetermined pH range, and the aqueous liquid is attached to a synthetic fiber filament strand subjected to contact heating type false twisting, whereby the lubricant and the water are brought into respective predetermined ratios.
Description
The invention relates to lubricating endowing method for the synthetic fiber filament strand of contact heating type false twisting processing.The synthetic fiber filament strand is carried out false twisting add man-hour, generally being to use heter temperature is installed is that 150-250 ℃, heater length are that heater, the synthetic fiber filament strand one side of 120-300cm contact the mobile contact heating type false twisting machine of one side with heating plate.With such contact heating type false twisting machine the synthetic fiber filament strand is carried out false twisting and add man-hour, for preventing fluffing or broken string, obtaining high-quality false twist yarn, it is important to prevent that the heater pollution from causing the pass.The present invention is exactly about preventing the lubricating endowing method of the synthetic fiber filament strand that this class heater pollutes effectively.
In the past, prevent the lubricating endowing method of the synthetic fiber filament strand that above-mentioned heater pollutes, be to adopt on the synthetic fiber filament strand for false twisting processing to adhere to the mixture of polyether compound and polyorganosiloxane compounds as lubricant always.In the method for this class prior art, the polyorganosiloxane compounds that mixes with polyether compound uses following compounds: 1) 25 ℃ viscosity is 30 * 10
-6m
2Above and 25 ℃ the surface tension of/s is at the dimethyl silicone polymer or the alkyl fluoride modification poly dimethyl polysiloxanes (spy opens clear 54-46923) of 28 dyne/below the cm; 2) 30 ℃ viscosity is 15 * 10
-6m
2The dimethyl silicone polymer (spy opens clear 48-53093) that/s is above; 3) 30 ℃ viscosity is 10 * 10
-6-80 * 10
-6m
2The phenyl polysiloxane of/s (special public clear 47-50657, US3756972); Perhaps 4) polyether modified siloxane (special public clear 63-57548, US4561987) etc.But the method for these prior aries can not prevent fully that the heater in the contact heating type false twisting processing from polluting.And if can not prevent fully that heater from polluting, fluffing or fracture of wire etc. will take place, thereby can not obtain high-quality false twist yarn.
The objective of the invention is, the solution art methods can not fully prevent the heater pollution problems in the contact heating type false twisting processing of synthetic fiber filament strand.
For this reason, the inventor has studied the lubricating endowing method that can fully prevent the synthetic fiber filament strand that heater pollutes in the contact heating type false twisting processing of synthetic fiber filament strand, found that, the lubricant of specific composition or the pH value of water-based liquid that contains the finishing agent of this lubricant are adjusted in the prescribed limit, adhere to this water-based liquid for synthetic fiber filament strand for contact heating type false twisting processing, make lubricant and moisture content reach the ratio of regulation respectively, just can address the above problem.
Promptly, the invention relates to lubricating endowing method for the synthetic fiber filament strand of contact heating type false twisting processing, it is characterized in that, the water-based liquid of following lubricant is adjusted to pH7-9, adhere to this water-based liquid for synthetic fiber filament strand for contact heating type false twisting processing, the ratio that makes lubricant is 0.1-3% (weight), and the ratio of moisture content is 0.2-10 a times of lubricant adhesion amount.
In addition, the invention relates to lubricating endowing method for the synthetic fiber filament strand of contact heating type false twisting processing, it is characterized in that, to be adjusted to pH7-9 by the water-based liquid that following lubricant and aliphatic epoxide constitute and per 100 parts of (weight) lubricants contain the finishing agent of 5 parts of (weight) following aliphatic epoxides, adhere to this water-based liquid for synthetic fiber filament strand for contact heating type false twisting processing, make lubricant reach the ratio of 0.1-3% (weight), and moisture content reach the 0.2-10 ratio doubly of lubricant adhesion amount.
Lubricant: by polyether compound be selected from that the linear polysiloxane more than a kind or 2 kinds among following linear polysiloxane A and the linear polysiloxane B constitutes and per 100 parts of (weight) polyether compounds contain the lubricant of the linear polysiloxane of 50 parts of (weight) following ratios.
Linear polysiloxane A: the linear polysiloxane that has 4-12 the siloxane unit shown in following 1 formula in the molecule as the repetitive that constitutes it.
Linear polysiloxane B: add up to as the repetitive that constitutes it in the molecule to have 4-12 the siloxane unit shown in following 1 formula and the siloxane unit shown in following 2 formulas and the siloxane unit shown in 2 formulas has the following ratio of 25% (mole) in whole siloxane units linear polysiloxane.
1 formula
2 formulas
In 1 formula and 2 formulas
R
1, R
2: identical or different alkyl with 1-4 carbon atom:
R
3: the fluoroalkyl of 1-4 carbon atom:
R
4: the alkyl of the fluoroalkyl of a 1-4 carbon atom or 1-4 carbon atom.
In the present invention, can use the linear polysiloxane more than a kind or 2 kinds that is selected among above-mentioned linear polysiloxane A and the linear polysiloxane B.
Linear polysiloxane A is to have 4-12 the siloxane unit shown in 1 formula as the repetitive that constitutes it in the molecule.Siloxane unit shown in 1 formula comprises: 1) the dialkylsiloxane unit that replaces with identical alkyl such as dimethyl siloxane units, di-ethyl siloxane unit, dipropyl siloxane unit, dibutyl siloxane unit; 2) the dialkylsiloxane unit that replaces with different alkyl such as Methylethyl siloxane unit, methyl butyl siloxane unit.It is dimethyl siloxane units person that linear polysiloxane A preferentially selects the siloxane unit shown in 1 formula for use, and wherein, especially preferentially selecting the whole siloxane units that constitute it for use is dimethyl siloxane units persons.
In addition, linear polysiloxane B is, adds up to as the repetitive that constitutes it in the molecule to have 4-12 siloxane unit shown in 1 formula and the siloxane unit shown in 2 formulas, and, in whole siloxane units, the siloxane unit shown in 2 formulas has the following ratio of 25% (mole).Siloxane unit shown in 1 formula is as top described, and the siloxane unit shown in 2 formulas comprises: 1) fluoroalkyl siloxane unit, 2) fluoroalkyl alkylsiloxane unit.Contained in such siloxane unit have a fluoroalkyl, except the alkyl that part fluorine such as γ-trifluoro propyl, beta, gamma-five fluoropropyl replace, can also enumerate the alkyl that perfluors such as octafluoro propyl group, pentafluoroethyl group replace.It is that the siloxane unit shown in dimethyl siloxane units, 2 formulas is the alkyl person that the part fluorine replaces that linear polysiloxane B preferentially selects the siloxane unit shown in 1 formula for use.In linear polysiloxane B, the siloxane unit shown in 2 formulas occupies the ratio below 25% (mole) in whole siloxane units, usually the ratio of 1-25% (mole) preferably.
The linear polysiloxane that uses among the present invention, in molecule, have 4-12 above-mentioned siloxane unit as the repetitive that constitutes it, preferably the carbon number that has an alkyl as end group is the trialkylsilkl of 1-3, such trialkylsilkl can be enumerated trimethyl silyl, triethylsilyl, trimethyl ethyl silicane base etc., wherein preferentially selects trimethyl silyl for use.In addition, these linear polysiloxane preferentially select for use the quantity of the repetitive that constitutes it to have the mixture of the linear polysiloxane of certain distribution, and when using such mixture, 25 ℃ viscosity is 3 * 10
-6-9 * 10
-6m
2The scope of/s, preferably 4 * 10
-6-8 * 10
-6m
2The scope of/s.
Can use known polyether compound with the polyether compound of linear polysiloxane and usefulness, for example special compound of being put down in writing among clear 56-31077, the special public clear 63-57548 etc. of opening.Such polyether compound can be enumerated, and the oxygen olefin unit that constitutes it is polyether polyol such as polyethers one alcohol, PTMEG, polyether triol of oxygen ethylene unit and oxypropylene unit.In the present invention, polyether compound is preferentially selected mean molecule quantity 700-20000 person for use.Polyether compound comprises the mixture of the polyether compound that molecular weight is different, when using such mixture, and the mixture of the polyether compound of preferential selection use mean molecule quantity 1000-3000 and the polyether compound of mean molecule quantity 5000-15000.
Aliphatic epoxide with linear polysiloxane and polyether compound and usefulness, can use known aliphatic epoxide, preferentially select the epoxides that is dissolved in water-based liquid described below for use, for example can enumerate: 1) oxirane, expoxy propane, 1, epoxyalkane such as 2-epoxy butane; 2) glycidol; 3) glycidol ether of polyalcohol such as ethylene glycol bisthioglycolate Synthesis of Oligo Ethylene Glycol, glycerol diglycidyl ether; 4) glycidol ether of polyether polyol such as polyethyleneglycol diglycidylether, poly-hydroxyethyl trihydroxymethylpropanyltri diglycidyl ether.
The lubricant that the present invention uses, constitute by polyether compound and the linear polysiloxane shown in top, and, with respect to 100 parts of (weight) polyether compounds, the content of linear polysiloxane is below 50 parts (weight), preferably 1-15 part (weight).In addition, the finishing agent that the present invention uses, be by such lubricant and top shown in aliphatic epoxide constitute, and, with respect to 100 parts of (weight) lubricants, the content of aliphatic epoxide below 5 parts (weight), 1-4 part (weight) preferably.
In the present invention, on the synthetic fiber filament strand of water-based liquid with above-mentioned lubricant or finishing agent attached to the processing of confession contact heating type false twisting.The aqueous solvent that uses during preparation water-based liquid can be enumerated water, water/pure mixed solvent, water/water-soluble ketone mixed solvent etc., preferentially selects water for use.Water-based liquid is modulated into lubricant or finishing agent and is dissolved in the emulsion that the aqueous solution that forms in the above-mentioned water-soluble solvent or emulsification form, and is being modulated into the occasion of emulsion, in order to obtain emulsion stability, can suitably select, use a small amount of as far as possible emulsifying agent.
Employed water-based liquid is adjusted to pH7-9, preferably pH8-9.In the present invention, the pH value is to measure by the method for JIS-Z8802.Usually, lubricant or finishing agent are adjusted to pH7-9 with the pH regulator agent with it being faintly acid without any processing its pH value under situation less than 6, preferably are adjusted to 8-9.In this occasion, the pH regulator agent can be added in lubricant or the finishing agent in advance, perhaps also it can be added in their the water-based liquid through adjustment.Can use known pH regulator agent, preferentially select following pH regulator agent for use: 1) octyldimethyl amine oxide, lauryl dimethyl amine oxide, N-octyl group morpholine oxide etc. has the aliphatic tertiary amine oxide of the aliphatic alkyl of 8-18 carbon atom, 2) isostearic acid dibutyl ethanolamine salt, triethanol amine oleates etc. have the monocarboxylic amine salt of aliphatic of the aliphatic alkyl of 8-18 carbon atom, 3) ten pentaene base butanedioic acid triethanolamine salts, octadecylene base butanedioic acid triethanolamine salt etc. has the amine salt of the aliphatic alkyl of 8-18 carbon atom as substituent replacement aliphatic dicarboxylic acid, is selected from above-mentioned 1)-3) in the alkali compounds more than a kind or 2 kinds.
In the present invention, for synthetic fiber filament strand, by lubricant 0.1-3% (weight), preferably the ratio of 0.2-1% (weight) and 0.2-10 that moisture content is the lubricant adhesion amount are doubly, preferably 2-8 times ratio is adhered to above-mentioned water-based liquid for contact heating type false twisting processing.In the present invention, the adhesion amount of moisture content is the numerical value of measuring by the method for JIS-K0068.Lubricant and moisture content can be regulated with known method with respect to the adhesion amount of synthetic fiber filament strand, promptly regulate the coiling speed of amounts of lubrication in the water-based liquid and moisture content amount and the silk in the spinning process of synthetic fiber filament strand etc.The water-based liquid that adopts water to be modulated into as aqueous solvent, if with cylinder to oil process with lubricant concentration 3-30% (weight), preferably the water-based liquid of 5-15% (weight) coiling speed that is attached in the spinning process silk is on the synthetic fiber filament strand that divides of 2500-7500m/, the adhesion amount of lubricant and moisture content can be adjusted to desirable numerical value.According to circumstances, when the adhesion amount deficiency of moisture content, can also carry out the second time, only adhere to moisture content.
In the present invention, on the synthetic fiber filament strand of the water-based liquid that is adjusted to pH7-9 with above-mentioned lubricant or finishing agent attached to the processing of confession contact heating type false twisting, usually, be attached on the synthetic fiber filament strand after just having spun in the spinning process with water-based liquid, batch the synthetic fiber filament strand that has adhered to water-based liquid, then the synthetic fiber filament strand that batches is supplied with contact heating type false twisting processing.The synthetic fiber filament strand that has adhered to water-based liquid according to the difference of the condition of batching, can obtain undrawn yarn, partially drawn yarn or drawn yarn, preferentially is chosen in the partially drawn yarn or the drawn yarn that obtain under the coiling speed of 2500-7500m/ branch in the present invention.
As mentioned above, the present invention is by adhering to the water-based liquid that is adjusted to pH7-9 of lubricant or finishing agent for the synthetic fiber filament strand, make lubricant and moisture content reach the ratio of regulation, can give synthetic fiber filament strand good lubricity, can prevent that therefore the heater in the contact heating type false twisting process from polluting for contact heating type false twisting processing.Contact heating type false twisting processing uses usually heter temperature that the twisting side is installed as 150-250 ℃, the heater of heater length 120-300cm, make synthetic fiber filament strand one side contact simultaneously mobile contact heating type false twisting machine with heating plate, wherein, the false twisting machine that use is equipped with the direct contact heater of twisting heter temperature 180-230 ℃ of side, heater length 150-250cm carries out contact heating type false twisting and adds man-hour, better effects if of the present invention.
In the present invention, for above-mentioned water-based liquid is had no particular limits attached to the method on the synthetic fiber filament strand, such adherence method can be enumerated cylinder and give oil process, spraying to known method such as oil processes for oil process, dipping for the deflector roll of oil process, use measuring pump, preferentially selects for use cylinder to give oil process for the deflector roll of oil process or use measuring pump.
The synthetic fiber filament strand that the present invention is suitable for can be enumerated: 1) be the polyester filament strand of main composition unit with the ethylene glycol terephthalate, 2) polyamide filaments strand such as nylon 6, nylon 66,3) polyacrylic acid such as polyacrylonitrile, modacrylic long filament strand, 4) polyolefin filaments such as polyethylene, polypropylene strand, wherein, when being used for polyester filament strand, polyamide filaments strand, effect is relatively good, when being used for polyester portion drawn yarn, polyamide partially drawn yarn and polyester direct spinning stretching silk, better effects if.
The working of an invention scheme
As embodiment of the present invention, can enumerate the following examples 1)-13).
1) will be as following (L-1) of lubricant 100 parts (weight), mix as the octyldimethyl amine oxide (C-1) of pH regulator agent 3 parts (weight) with as polyethylene glycol oxide (7 moles) nonylplenyl ethers (E-1) 3 parts (weight) of emulsifying agent, in this mixture (M-1), add 1322 parts of (weight) water and diluted, make be adjusted to pH8.5, lubricant (L-1) concentration is the water-based liquid of 7% (weight).With this water-based liquid attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 3300m/ divides, obtaining lubricant (L-1) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 1 times polyester filament partially drawn yarn of lubricant (L-1) adhesion amount.Then, this polyester filament partially drawn yarn is supplied with contact heating type false twisting processing.
(L-1): the lubricant that will form by the polyether compound (P-1) of the mean molecule quantity 4250 of the composition of proportions of polyalkylene glycols ether=50/50 (weight ratio) of the butoxy polyalkylene glycols ether/mean molecule quantity 7000 of mean molecule quantity 1500 and following linear polysiloxane (A-1), by the mixed of polyether compound (P-1)/linear polysiloxane (A-1)=100/10 (weight ratio).
Linear polysiloxane (A-1): in the molecule as the repetitive that constitutes it have 8 dimethyl siloxane units, as its not end group have the linear polysiloxane of trimethyl silyl.
2) above-mentioned 1) (M-1) in further mix 1 part of diethylene glycol (DEG) diglycidyl ether (D-1) (weight) as aliphatic epoxide, in this mixture, add 1321 parts of (weight) water and diluted, make be adjusted to pH8.5, lubricant (L-1) concentration is the water-based liquid of 7% (weight).With this water-based liquid attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 3300m/ divides, obtaining lubricant (L-1) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 1 times polyester filament partially drawn yarn of lubricant (L-1) adhesion amount.Then, this polyester filament partially drawn yarn is supplied with contact heating type false twisting processing.
3) will as following (L-2) of lubricant 100 parts (weight), as the isostearic acid dibutyl ethanolamine salt (C-2) of pH regulator agent 3 parts (weight) and as emulsifying agent above-mentioned 1) (E-1) 3 parts (weight) mix, in this mixture (M-2), add 3227 parts of (weight) water and diluted, make be adjusted to pH8.7, lubricant (L-2) concentration is the water-based liquid of 3% (weight).With this water-based liquid attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 3300m/ divides, obtaining lubricant (L-2) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 2 times polyester filament partially drawn yarn of lubricant (L-2) adhesion amount.Then, this polyester filament partially drawn yarn is supplied with contact heating type false twisting processing.
(L-2): the lubricant that above-mentioned polyether compound (P-1) and following polysiloxane (A-2) are formed by the mixed of polyether compound (P-1)/polysiloxane (A-2)=100/5 (weight ratio).
Polysiloxane (A-2): have 11 dimethyl siloxane units, have the polysiloxane of trimethyl silyl as its end group as the repetitive that constitutes it in the molecule.
4) above-mentioned 3) (M-2) in, further mix 1 part of glycidol (D-2) (weight) as aliphatic epoxide, the water that adds 3226 parts (weight) in this mixture is diluted, make be adjusted to pH8.7, lubricant (L-2) concentration is the water-based liquid of 3% (weight).With this water-based liquid attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 3300m/ divides, obtaining lubricant (L-2) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 2 times polyester filament partially drawn yarn of lubricant (L-2) adhesion amount.Then, this polyester filament partially drawn yarn is supplied with contact heating type false twisting processing.
5) will as following (L-3) of lubricant 100 parts (weight), as ten pentaene base butanedioic acid triethanolamine salts (C-3) of pH regulator agent 3 parts (weight) and as emulsifying agent above-mentioned 1) (E-1) 3 parts (weight) mix, in this mixture (M-3), add 1894 parts of (weight) water and diluted, make be adjusted to pH8.8, lubricant (L-3) concentration is the water-based liquid of 5% (weight).With this water-based liquid attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 3300m/ divides, obtaining lubricant (L-3) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 1.5 times polyester filament partially drawn yarn of lubricant (L-3) adhesion amount.Then, this polyester filament partially drawn yarn is supplied with contact heating type false twisting processing.
(L-3): the lubricant that will form by the polyether compound (P-2) of the mean molecule quantity 2350 of the composition of proportions of polyalkylene glycols ether=90/10 (weight ratio) of the butoxy polyalkylene glycols ether/mean molecule quantity 10000 of mean molecule quantity 1500 and following linear polysiloxane (B-1), by the mixed of polyether compound (P-2)/linear polysiloxane (B-1)=100/7 (weight ratio).
Linear polysiloxane (B-1): have 5 dimethyl siloxane units and 1 methyl γ-trifluoropropyl siloxane unit, have the linear polysiloxane of trimethyl silyl as its end group as the repetitive that constitutes it in the molecule.
6) above-mentioned 3) (M-2) in, further mix 1 part of glycerol diglycidyl ether (D-3) (weight) as aliphatic epoxide, the water that adds 2394 parts (weight) in this mixture is diluted, make be adjusted to pH8.8, lubricant (L-2) concentration is the water-based liquid of 5% (weight).With this water-based liquid attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 3300m/ divides, obtaining lubricant (L-2) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 1.5 times polyester filament partially drawn yarn of lubricant (L-2) adhesion amount.Then, this polyester filament partially drawn yarn is supplied with contact heating type false twisting processing.
7) with above-mentioned 1) in preparation, lubricant (L-1) concentration is that the water-based liquid of 7% (weight) is attached on the intact Tynex strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 4200m/ divides, obtaining lubricant (L-1) adhesion amount is that 0.45% (weight), moisture content adhesion amount are 1.5 times Tynex partially drawn yarn of lubricant (L-1) adhesion amount.Then, this Tynex partially drawn yarn is supplied with contact heating type false twisting processing.
8) with above-mentioned 2) in preparation, lubricant (L-1) concentration is that the water-based liquid of 7% (weight) is attached on the intact Tynex strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 4200m/ divides, obtaining lubricant (L-1) adhesion amount is that 0.45% (weight), moisture content adhesion amount are 1.5 times Tynex partially drawn yarn of lubricant (L-1) adhesion amount.Then, this Tynex partially drawn yarn is supplied with contact heating type false twisting processing.
9) with above-mentioned 5) in preparation, lubricant (L-3) concentration is that the water-based liquid of 5% (weight) is attached on the intact Tynex strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 4200m/ divides, obtaining lubricant (L-3) adhesion amount is that 0.45% (weight), moisture content adhesion amount are 3 times Tynex partially drawn yarn of lubricant (L-3) adhesion amount.Then, this Tynex partially drawn yarn is supplied with contact heating type false twisting processing.
10) with above-mentioned 6) in preparation, lubricant (L-2) concentration is that the water-based liquid of 5% (weight) is attached on the intact Tynex strand of spinning just in the spin-drawing coiling process, batch with the coiling speed that 4200m/ divides, obtaining lubricant (L-2) adhesion amount is that 0.45% (weight), moisture content adhesion amount are 3 times Tynex partially drawn yarn of lubricant (L-2) adhesion amount.Then, this Tynex partially drawn yarn is supplied with contact heating type false twisting processing.
11) with above-mentioned 2) in preparation, lubricant (L-1) concentration is that the water-based liquid of 7% (weight) is attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, the rotary speed of dividing with 3800m/ with the 1st godet roller is drawn and is got, mechanical stretching between the 2nd godet roller again, batch with the coiling speed that 6000m/ divides, obtaining lubricant (L-1) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 1 times polyester filament direct spinning stretching silk of lubricant (L-1) adhesion amount.Then, this polyester filament direct spinning stretching silk is supplied with contact heating type false twisting processing.
12) with above-mentioned 4) in preparation, lubricant (L-2) concentration is that the water-based liquid of 3% (weight) is attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, the rotary speed of dividing with 3800m/ with the 1st godet roller is drawn and is got, mechanical stretching between the 2nd godet roller again, batch with the coiling speed that 6000m/ divides, obtaining lubricant (L-2) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 3 times polyester filament direct spinning stretching silk of lubricant (L-2) adhesion amount.Then, this polyester filament direct spinning stretching silk is supplied with contact heating type false twisting processing.
13) with above-mentioned 5) in preparation, lubricant (L-3) concentration is that the water-based liquid of 5% (weight) is attached on the intact polyester filament strand of spinning just in the spin-drawing coiling process, the rotary speed of dividing with 3800m/ with the 1st godet roller is drawn and is got, mechanical stretching between the 2nd godet roller again, batch with the coiling speed that 6000m/ divides, obtaining lubricant (L-3) adhesion amount is that 0.4% (weight), moisture content adhesion amount are 2 times polyester filament direct spinning stretching silk of lubricant (L-3) adhesion amount.Then, this polyester filament direct spinning stretching silk is supplied with contact heating type false twisting processing.
Below, enumerate embodiment and comparative example and be described more specifically formation of the present invention and effect, but the present invention is not subjected to the restriction of these embodiment.In addition, in following embodiment and comparative example, described part is meant that weight portion, % are meant weight %.
Embodiment
Test 1 (preparation water-based liquid)
Preparation water-based liquid (T-1)
Will be by butoxy polyalkylene glycols ether (oxygen ethylene unit/oxypropylene unit=70/30 (mol ratio), random addition, mean molecule quantity 1500)/polyalkylene glycols ether (oxygen ethylene unit/oxypropylene unit=20/80 (mol ratio), random addition, mean molecule quantity 7000)=50/50 have 8 dimethyl siloxane units as the repetitive that constitutes it in the polyether compound (P-1) of the mean molecule quantity 4250 of (weight ratio) formation and the molecule, the linear polysiloxane (A-1) that has trimethyl silyl as its end group, press the mixed of polyether compound (P-1)/linear polysiloxane (A-1)=100/10 (weight ratio), make lubricant (L-1).In 100 parts of these lubricants (L-1), add 3 parts of octyldimethyl amine oxides (C-1) as the pH regulator agent, as 1322 parts in 3 parts of polyoxyethylene (7 moles) nonylplenyl ethers (E-1) of emulsifying agent and water, adjusted to pH8.5, lubricant (L-1) concentration is 1428 parts of 7% water-based liquid (T-1).
Preparation water-based liquid (T-2)～(T-6), (TR-1)～(TR-11)
Same with water-based liquid (T-1), preparation water-based liquid (T-2)～(T-6), (TR-1)～(TR-11).Comprise water-based liquid (T-1), the composition of these water-based liquid etc. gathers and is shown in Table 1.In addition, the composition that is used to prepare the lubricant of these water-based liquid gathers and is shown in Table 2.
Table 1
| The kind of water-based liquid | The composition of water-based liquid | The concentration of water-based liquid | The pH of water-based liquid | ||||||||
| Lubricant | The pH regulator agent | The aliphatic epoxy compound | Emulsifying agent | The consumption of water | |||||||
| Kind | Consumption | Kind | Consumption | Kind | Consumption | Kind | Consumption | ||||
| ??T-1 ??T-2 ??T-3 ??T-4 ??T-5 ??T-6 | ??L-1 ??L-1 ??L-2 ??L-2 ??L-3 ??L-3 | ?100 ?100 ?100 ?100 ?100 ?100 | ?C-1 ?C-1 ?C-2 ?C-2 ?C-3 ?C-3 | ??3 ??3 ??3 ??3 ??3 ??3 | ??D-1 ??D-2 ??D-3 | ???1 ???1 ???1 | ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 | ???3 ???3 ???3 ???3 ???3 ???3 | ??1322 ??1321 ??3227 ??3226 ??1894 ??2394 | ???7.0 ???7.0 ???3.0 ???3.0 ???5.0 ???5.0 | ???8.5 ???8.5 ???8.7 ???8.7 ???8.8 ???8.8 |
| ??TR-1 ??TR-2 ??TR-3 ??TR-4 ??TR-5 ??TR-6 ??TR-7 ??TR-8 ??TR-9 ??TR-10 ??TR-11 | ??L-1 ??L-2 ??L-3 ??LR-1 ??LR-2 ??LR-3 ??LR-4 ??LR-5 ??LR-6 ??L-1 ??L-1 | ?100 ?100 ?100 ?100 ?100 ?100 ?100 ?100 ?100 ?100 ?100 | ?B-1 ?B-4 ?B-1 | ??3 ??3 ??3 | ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 ?E-1 | ???3 ???3 ???3 ???3 ???3 ???3 ???3 ???3 ???3 ???3 ???3 | ??1325 ??3230 ??1897 ??1325 ??3230 ??1897 ??1325 ??1325 ??1322 ??1322 ??3227* ??1 | ???7.0 ???3.0 ???5.0 ???7.0 ???3.0 ???5.0 ???7.0 ???7.0 ???7.0 ???7.0 ???3.0 | ???6.0 ???6.0 ???6.0 ???6.0 ???6.0 ???6.0 ???6.0 ???6.0 ???8.5 ??10.5 ???8.5 | ||
In table 1,
Use amount: unit is part
Concentration: unit is %
L-1～L-3, LR-1～L R-6: the lubricant shown in the table 2
C-1: octyldimethyl amine oxide
C-2: isostearic acid dibutyl ethanolamine salt
C-3: ten pentaene base butanedioic acid triethanolamine salts
C-4: sodium carbonate
D-1: diethylene glycol (DEG) diglycidyl ether
D-2: glycidol
D-3: glycerol diglycidyl ether
E-1: polyoxyethylene (7 moles) nonylplenyl ether
* 1: make the mixed solvent of water/isopropyl alcohol=3/97 (weight ratio) replace water
Table 2
| The lubricant kind | Polyether compound | Polysiloxane | Polyether compound/linear polysiloxane (weight ratio) | |||||||||
| Kind | Consumption (part) | Kind | The siloxane unit of 1 formula | The siloxane unit of 2 formulas | End group | Viscosity | Consumption (part) | |||||
| Kind | Number of repetition | Kind | Number of repetition | Kind | Quantity | |||||||
| ?L-1 ?L-2 ?L-3 | ?P-1 ?P-1 ?P-2 | ?100 ?100 ?100 | ??A-1 ??A-2 ??B-1 | ??DM-1 ??DM-1 ??DM-1 | ????8 ????11 ????5 | ??MF-1 | ???1 | ???TM-1 ???TM-1 ???TM-1 | ????2 ????2 ????2 | ???5.0 ???7.5 ???5.0 | ??10 ???5 ???7 | ??100/10 ??100/5 ??100/7 |
| ?LR-1 ?LR-2 ?LR-3 ?LR-4 ?LR-5 ?LR-6 | ?P-1 ?P-1 ?P-2 ?P-1 ?P-1 ?P-1 | ?100 ?100 ?100 ?100 ?100 ?100 | ??AR-1 ??AR-2 ??BR-1 ??AR-3 ???R-1 ???A-1 | ??DM-1 ??DM-1 ??DM-1 ??DM-1 | ????2 ????16 ????16 ????8 | ??MF-1 | ???1 | ???TM-1 ???TM-1 ???TM-1 ???TM-1 | ????2 ????2 ????2 ????2 | ???1.5 ???15.0 ???18.0 ???40.0 ???750.0 ???5.0 | ??10 ???5 ???7 ??10 ???5 ??75 | ??100/10 ??100/5 ??100/7 ??100/10 ??100/5 ??100/75 |
In table 2,
Viscosity: 25 ℃ viscosity, unit is 1 * 10
-6m
2/ s
P-1: be to be that the random addition product of 1500 butoxy polyalkylene epoxy propyl ether and oxygen ethylene unit/oxypropylene unit=20/80 (mol ratio) and mean molecule quantity are 7000 polyalkylene epoxy propyl ether, the polyether compound of the mean molecule quantity 4250 that obtains by the mixed of 50/50 (weight ratio) with the random addition product of oxygen ethylene unit/oxypropylene unit=70/30 (mol ratio) and mean molecule quantity
P-2: be to be that the random addition product of 1500 butoxy polyalkylene epoxy propyl ether and oxygen ethylene unit/oxypropylene unit=25/75 (mol ratio) and mean molecule quantity are 10000 polyalkylene epoxy propyl ether by the polyether compound of, the mean molecule quantity 2350 that obtains by the mixed of 90/10 (weight ratio) with the random addition product of oxygen ethylene unit/oxypropylene unit=60/40 (mol ratio) and mean molecule quantity
A-1: have 8 dimethyl siloxane units, have the linear polysiloxane of trimethyl silyl as its end group as the repetitive that constitutes it in the molecule
A-2: have 11 dimethyl siloxane units, have the linear polysiloxane of trimethyl silyl as its end group as the repetitive that constitutes it in the molecule
B-1: have 5 dimethyl siloxane units and 1 methyl γ-trifluoropropyl siloxane unit, have the linear polysiloxane of trimethyl silyl as its end group as the repetitive that constitutes it in the molecule
AR-1: have 2 dimethyl siloxane units, have the linear polysiloxane of trimethyl silyl as its end group as the repetitive that constitutes it in the molecule
AR-2: have 16 dimethyl siloxane units, have the linear polysiloxane of trimethyl silyl as its end group as the repetitive that constitutes it in the molecule
AR-3: in the molecule as the repetitive that constitutes it have n dimethyl siloxane units, mean molecule quantity is 3000 linear polysiloxane
BR-1: have 16 dimethyl siloxane units and 1 methyl γ-trifluoropropyl siloxane unit, have the linear polysiloxane of trimethyl silyl as its end group as the repetitive that constitutes it in the molecule
R-1: the polyether-modified polysiloxanes of mean molecule quantity 8600, polyoxyalkylene ether block contain proportional be 92% and this polyoxyalkylene ether block be the polyether-modified polysiloxanes of the random addition product of oxygen ethylene unit/oxypropylene unit=50/50 (mol ratio)
DM-1: dimethyl siloxane units
MF-1: methyl γ-trifluoropropyl siloxane
TM-1: trimethyl silyl
2 (on the polyester filament strand, adhering to water-based liquid and evaluation thereof) of test
With conventional method with inherent viscosity be 0.64, titanium oxide content is 0.6% polyethylene terephthalate chip drying, uses extruder type spinning machine 295 ℃ of following spinning then.To test each water-based liquid of obtaining in 1 to oil process with cylinder attached on the mobile strand behind spinning nozzle ejection, cooling curing, batch with the speed that 3300m/ divides, obtain with respect to the lubricant adhesion amount of strand and the 10kg winding cake of attachment of moisture amount polyester filament partially drawn yarns as shown in table 3,75 DENIER, 72 threads.Carry out false twisting processing with this polyester filament partially drawn yarn by following described false twisting processing conditions, the heater of estimating in the false twisting process pollutes.The results are shown in the table 3.
The false twisting processing conditions
Use contact heating type false twisting machine (SDS-1200B that ア-ネ ス ト ス Network ラ Star グ ア Application De サ Application ズ company makes), continuously running 21 days under following condition is carried out false twisting processing: process velocity=820m/ branch, draw ratio=1.519, surface temperature=215 ℃ of executing sth. made by twisting mode=3 a disk circumscribed friction mode (1 in input side guide wheel disk, 1 in outlet side guide wheel disk, 7 in hard polyaminoester disk), twisting side heater length=2.5m, twisting side heater, backtwisting side heater=nothing, target twisting count=3350T/m.
The evaluation that heater pollutes: after turning round continuously 21 days under these conditions, the heater tar bruss that will twist with brush on the silk road of side heater surfaces gets off, and is collected in weighing afterwards together.The result measures, represents with the average weight (mg) of per 1 spindle 10 spindles.
Table 3
| Distinguish | Water-based liquid | The adhesion amount of lubricant | The adhesion amount of moisture (doubly) | The evaluation (mg) that heater pollutes | |
| Kind | ???pH | ????(％) | |||
| Embodiment 123456 | ???T-1 ???T-2 ???T-3 ???T-4 ???T-5 ???T-6 | ???8.5 ???8.5 ???8.7 ???8.7 ???8.8 ???8.8 | ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 | ????1.0 ????1.0 ????2.0 ????2.0 ????1.5 ????1.5 | ?????75 ?????65 ?????80 ?????80 ?????100 ?????95 |
| Comparative example 123456789 10 11 12 | ???TR-1 ???TR-2 ???TR-3 ???TR-4 ???TR-5 ???TR-6 ???TR-7 ???TR-8 ???TR-9 ???TR-10 ???TR-11 ???T-6 | ???6.0 ???6.0 ???6?0 ???6.0 ???6.0 ???6.0 ???6.0 ???6.0 ???8.5 ??10.5 ???8.5 ???8.5 | ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 ?????0.4 | ????1.0 ????2.0 ????1.5 ????1.0 ????2.0 ????1.5 ????1.0 ????1.0 ????1.0 ????1.0 ????0.1 ???12.0 | ?????460 ?????550 ?????580 ?????1700 ?????760 ?????630 ?????690 ?????410 ?????1050 ?????460 ?????380 ?????*3 |
In table 3,
The adhesion amount of lubricant: before false twisting processing beginning, with respect to the lubricant adhesion amount (%) of polyester filament partially drawn yarn
The adhesion amount of moisture: before false twisting processing beginning, with respect to attachment of moisture amount (doubly) attached to the lubricant adhesion amount on the polyester filament partially drawn yarn
Comparative example 12: on mobile strand, adhere to water-based liquid, and then attached water
* 3: broken string is many, can not turn round continuously
Test 3 (on Tynex is long, adhering to water-based liquid and evaluation thereof)
With conventional method with sulfuric acid relative viscosity η r be 2.4, titanium oxide content is 0.4 nylon 6,6 chip dryings, uses extruder type spinning machine 29 ℃ of following spinning then.To test each water-based liquid of obtaining in 2 to oil process with deflector roll attached on the mobile strand behind spinning nozzle ejection, cooling curing, batch in the speed that does not have to divide with 4200m/ under the situation of mechanical stretching, obtain with respect to the lubricant adhesion amount of strand and the 8kg winding cake of attachment of moisture amount Tynex partially drawn yarns as shown in table 4,30 DENIER, 12 threads.Carry out false twisting processing with this Tynex partially drawn yarn by following described false twisting processing conditions, pollute with the test 2 same heaters of estimating in the false twisting process.The results are shown in the table 4.
The false twisting processing conditions
Use and test 2 same contact heating type false twisting machines, the following running continuously of following condition 21 days, carry out false twisting processing: process velocity=900m/ branch, draw ratio=1.215, surface temperature=215 ℃ of executing sth. made by twisting mode=3 a disk circumscribed friction mode (1 in input side guide wheel disk, 1 in outlet side guide wheel disk, 5 of ceramic disk), twisting side heater length=2.5m, twisting side heater, backtwisting side heater=nothing, target twisting count=3100T/m.
Table 4
| Distinguish | Water-based liquid | The adhesion amount of lubricant | The adhesion amount of moisture (doubly) | The evaluation (mg) that heater pollutes | |
| Kind | ????pH | ????(％) | |||
| Embodiment 789 10 | ???T-1 ???T-2 ???T-5 ???T-6 | ???8.5 ???8.5 ???8.8 ???8.8 | ????0.45 ????0.45 ????0.45 ????0.45 | ????1.5 ????1.5 ????3.0 ????3.0 | ????100 ????140 ????65 ????90 |
| Comparative example 13 14 15 16 17 18 19 20 21 22 23 | ???TR-1 ???TR-3 ???TR-4 ???TR-5 ???TR-6 ???TR-7 ???TR-8 ???TR-9 ???TR-10 ???TR-11 ???T-5 | ???6.0 ???6.0 ???6.0 ???6.0 ???6.0 ???6.0 ???6.0 ???8.5 ???10.5 ???8.5 ???8.5 | ????0.45 ????0.45 ????0.45 ????0.45 ????0.45 ????0.45 ????0.45 ????0.45 ????0.45 ????0.45 ????0.45 | ????1.5 ????3.0 ????1.5 ????5.0 ????3.0 ????1.5 ????1.5 ????1.5 ????1.5 ????0.1 ????12.0 | ????630 ????600 ????1850 ????620 ????590 ????550 ????430 ????2650 ????570 ????460 ????*4 |
In table 4,
The adhesion amount of lubricant: before false twisting processing beginning, with respect to the lubricant adhesion amount (%) of Tynex partially drawn yarn
The adhesion amount of moisture: before false twisting processing beginning, with respect to attachment of moisture amount (doubly) attached to the lubricant adhesion amount on the Tynex partially drawn yarn
Comparative example 23: on mobile strand, adhere to water-based liquid, and then attached water
* 4: broken string is many, can not turn round continuously
4 (on the polyester filament strand, adhering to water-based liquid and evaluation thereof) of test
To test the water-based liquid that obtains in 1 with deflector roll to oil process moves on the strand attached to polyester filament, the 1st godet roller that the speed of dividing in order to 3800m/ is rotated draws to be got, mechanical stretching between the 2nd godet roller again, batch with the speed that 6000m/ divides, the adhesion amount that obtains lubricant for polyester filament direct spinning stretching silk is that the adhesion amount of 0.4% (weight), moisture is 5kg winding cakes numerical value shown in the table 5,50 DENIER, 36 threads.Use this polyester filament direct spinning stretching silk, except draw ratio 1.519 being changed into the super fear rate 3%,, use the heater of estimating in the false twisting process with the 2 same methods of testing to pollute according to carrying out false twisting processing with the same false twisting processing conditions of test 2.The results are shown in the table 5.
Table 5
| Distinguish | Water-based liquid | The adhesion amount of lubricant (%) | The adhesion amount of moisture (doubly) | The evaluation (mg) that heater pollutes | |
| Kind | ??pH | ||||
| Embodiment 11 12 13 | ??T-2 ??T-4 ??T-5 | ??8.5 ??8.7 ??8.8 | ????0.4 ????0.4 ????0.4 | ????1.0 ????3.0 ????2.0 | ????80 ????65 ????100 |
| Comparative example 24 25 26 27 28 29 | ??TR-1 ??TR-3 ??TR-4 ??TR-5 ??TR-9 ??TR-10 | ??6.0 ??6.0 ??6.0 ??6.0 ??8.5 ??10.5 | ????0.4 ????0.4 ????0.4 ????0.4 ????0.4 ????0.4 | ????1.0 ????2.0 ????1.0 ????3.0 ????1.0 ????1.0 | ????570 ????590 ????1750 ????1010 ????850 ????460 |
In table 5,
The adhesion amount of lubricant: before false twisting processing beginning, with respect to the lubricant adhesion amount (%) of polyester filament direct spinning stretching silk
The adhesion amount of moisture: before false twisting processing beginning, with respect to attachment of moisture amount (doubly) attached to the lubricant adhesion amount on the polyester filament direct spinning stretching silk
The effect of invention
As mentioned above, the present invention has the effect that can prevent fully that the heater of filament of synthetic fibre strand in the contact heating type false twisting process from polluting.
Claims (8)
1. supply the lubricating endowing method of the synthetic fiber filament strand of contact heating type false twisting processing, it is characterized in that, the water-based liquid of following lubricant is adjusted to pH7-9, adhere to this water-based liquid for synthetic fiber filament strand for contact heating type false twisting processing, the ratio that makes lubricant is 0.1-3% (weight), the ratio of moisture content be lubricant adhesion amount 0.2-10 doubly
Lubricant: by polyether compound be selected from that the linear polysiloxane more than a kind or 2 kinds among following linear polysiloxane A and the linear polysiloxane B constitutes and per 100 parts of (weight) polyether compounds contain the lubricant of the linear polysiloxane of 50 parts of (weight) following ratios;
Linear polysiloxane A: the linear polysiloxane that has 4-12 the siloxane unit shown in following 1 formula in the molecule as the repetitive that constitutes it;
Linear polysiloxane B: add up to as the repetitive that constitutes it in the molecule to have 4-12 the siloxane unit shown in following 1 formula and the siloxane unit shown in following 2 formulas and the siloxane unit shown in 2 formulas has the following ratio of 25% (mole) in whole siloxane units linear polysiloxane.
1 formula
2 formulas
In 1 formula and 2 formulas
R
1, R
2: identical or different alkyl with 1-4 carbon atom;
R
3: the fluoroalkyl of 1-4 carbon atom;
R
4: the alkyl of the fluoroalkyl of a 1-4 carbon atom or 1-4 carbon atom.
2. supply the lubricating endowing method of the synthetic fiber filament strand of contact heating type false twisting processing, it is characterized in that, to constitute by described lubricant of claim 1 and aliphatic epoxide, and the water-based liquid that per 100 parts of (weight) these lubricants contain the finishing agent of 5 parts of (weight) following aliphatic epoxides is adjusted to pH7-9, on the synthetic fiber filament strand of this water-based liquid attached to the processing of confession contact heating type false twisting, make with respect to synthetic fiber filament strand lubricant reach the ratio of 0.1-3% (weight), and moisture content reach the 0.2-10 ratio doubly of lubricant adhesion amount.
3. claim 1 or the 2 described lubricating endowing methods that supply the synthetic fiber filament strand of contact heating type false twisting processing is characterized in that lubricant is the lubricant that per 100 parts of (weight) petchems contain 1-15 part (weight) polysiloxane.
4. claim 1, the 2 or 3 described lubricating endowing methods that supply the synthetic fiber filament strand of contact heating type false twisting processing is characterized in that, with following pH regulator agent water-based liquid are adjusted to pH7-9,
PH regulator agent: be selected from the aliphatic tertiary amine oxide of aliphatic alkyl, the monocarboxylic amine salt of aliphatic of aliphatic alkyl and aliphatic alkyl with 8-18 carbon atom as the alkali compounds more than a kind or 2 kinds in the amine salt of substituent replacement aliphatic dicarboxylic acid with 8-18 carbon atom with 8-18 carbon atom.
5. claim 1,2, the 3 or 4 described lubricating endowing methods that supply the synthetic fiber filament strand of contact heating type false twisting processing is characterized in that the siloxane unit shown in 1 formula is a dimethyl siloxane units.
6. the lubricating endowing methods of claim 1,2,3,4 or 5 described synthetic fiber filament strands for contact heating type false twistings processing, it is characterized in that linear polysiloxane is that the carbon number that has an alkyl as end group is the trialkylsilkl of 1-3.
7. claim 1,2,3,4, the 5 or 6 described lubricating endowing methods that supply the synthetic fiber filament strand of contact heating type false twisting processing is characterized in that the mean molecule quantity of petchem is 700-20000.
8. the lubricating endowing methods of claim 1,2,3,4,5,6 or 7 described synthetic fiber filament strands for contact heating type false twistings processing, it is characterized in that polyether compound is the compound of mean molecule quantity 1000-3000 and the mixture of mean molecule quantity 5000-15000 compound.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP307218/96 | 1996-11-01 | ||
| JP30721896A JP3649422B2 (en) | 1996-11-01 | 1996-11-01 | Synthetic fiber filament processing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1182812A true CN1182812A (en) | 1998-05-27 |
Family
ID=17966472
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 97122873 Pending CN1182812A (en) | 1996-11-01 | 1997-11-01 | Method for imparting lubricity to synthetic fiber filament yarn subjected to contact heating type false twisting |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP3649422B2 (en) |
| CN (1) | CN1182812A (en) |
| ID (1) | ID17681A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101324028B (en) * | 2007-06-08 | 2013-05-29 | 竹本油脂株式会社 | Treating agent for synthetic fiber, synthetic fiber false-twist textured yarn, and treating method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8112980B2 (en) | 2007-09-10 | 2012-02-14 | Matsumoto Yushi-Seiyaku Co., Ltd. | Finish for synthetic filament yarn processed in friction false-twist texturing and application thereof |
-
1996
- 1996-11-01 JP JP30721896A patent/JP3649422B2/en not_active Expired - Fee Related
-
1997
- 1997-10-31 ID IDP973571A patent/ID17681A/en unknown
- 1997-11-01 CN CN 97122873 patent/CN1182812A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101324028B (en) * | 2007-06-08 | 2013-05-29 | 竹本油脂株式会社 | Treating agent for synthetic fiber, synthetic fiber false-twist textured yarn, and treating method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10131055A (en) | 1998-05-19 |
| ID17681A (en) | 1998-01-22 |
| JP3649422B2 (en) | 2005-05-18 |
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