CN106674515A - Method for preparing nylon 6 civil chips with uniform dyeing properties - Google Patents
Method for preparing nylon 6 civil chips with uniform dyeing properties Download PDFInfo
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- CN106674515A CN106674515A CN201710007964.2A CN201710007964A CN106674515A CN 106674515 A CN106674515 A CN 106674515A CN 201710007964 A CN201710007964 A CN 201710007964A CN 106674515 A CN106674515 A CN 106674515A
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- polyamide fibre
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/46—Post-polymerisation treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Abstract
The invention provides a method for preparing nylon 6 civil chips with uniform dyeing properties. The method includes steps of (1), melting solid caprolactam by the aid of an external heater, then mixing and uniformly stirring the caprolactam and auxiliaries with one another to obtain mixed liquid; (2), adding the mixed liquid prepared at the step (1) into a reaction kettle, carrying out polymerization reaction, discharging materials after the reaction is completely carried out, cooling the materials by the aid of water tanks and then granulating the materials; (3), extracting granules prepared at the step (2), then drying the granules and carrying out solid-phase viscosity increasing on the granules; (4), slicing finished products. The method for preparing the nylon 6 civil chips with the uniform dyeing properties has the advantages that the method is easy to implement, and spinning materials prepared from the nylon 6 civil chips are good in permeability and high in color fastness and can be uniformly dyed.
Description
Technical field
The present invention relates to textile technology field, more particularly to a kind of civilian section of level dyeing polyamide fibre 6 preparation method.
Background technology
Polyamide fibre 6 is the second largest chemical fibre of synthetic fibers, so either civilian or tool foot is all accounted on industrial
The status of weight.Nylon fibre for example can be made by polyamide fibre -6, and nylon fibre have compared with terylene, acrylic fibers it is many excellent
Point, such as solid wear-resisting, density is small, and fabric is light etc., the accreditation of consumer is especially obtained in light open air field, not only relaxed with warming
The characteristic such as suitable, also because different dyeabilities so that fabric possess how far color, but nylon fibre permeability is poor, dye
It is easily uneven during the material bad dyeing of adhesive force.
Such as Application No.：201010533168.0 Chinese patent disclose and a kind of prepare emerging film use using caprolactam
The production technology of nylon chips：The production technology is comprised the following steps：1) preparation of raw material caprolactam, 2) auxiliary agent and water standard
Standby, 3) prepolymerization, 4) polymerization, 5) pelletizing, 6) continuous extraction, 7) continuous drying and solid-phase tack producing, 8) viscous section high is modified, and 9) into
Product are cut into slices, and what this application was mainly produced is the section of high viscosity, but the section of high viscosity is difficult to be dyeed, and can cause dyeing
Uneven problem.
And for example Application No.：201310336802.5 Chinese patent disclose a kind of preparation method of chinlon 6 section, wrap
Include following steps：Caprolactam is dissolved into liquid, rutgers is added as initiator, and ultra-violet absorber,
Mixing and stirring；Liquid after stirring is added in reactor, nitrogen charging displaced air is heated slowly to 220~260
DEG C, 5~lOh is reacted with the mixing speed of 100~120r/min, discharge is simultaneously cut into slices after tank cooling, is cut into slices after being polymerized；
To cut into slices after polymerization with 80~100 DEG C of water hot extractions 30 hours, 50 DEG C of air blow drying surface moistures, section after must extracting；Will extraction
Section vacuum drying chamber obtains chinlon 6 section in 100~120 DEG C of 7~9h of drying after taking.Ultraviolet suction is added with this application
Agent is received, can effectively be prevented due to the COLOR FASTNESS PROBLEM of ultraviolet irradiation etc. after nylon dyeing, but easily cause dyestuff in process of production
Skewness, obtained spinning material dyeing quality is not good.
The content of the invention
During overcoming present in prior art using chinlon 6 section production nylon fibre, dye uneven etc.
Problem, the invention provides a kind of preparation method of the civilian section of level dyeing polyamide fibre 6.
Concrete technical scheme is as follows：
A kind of preparation method of the civilian section of level dyeing polyamide fibre 6, comprises the following steps：
Step (1)：Solid caprolactam is mixed and stirred for uniformly after external heater is melted with auxiliary agent；
Step (2)：Mixing liquid obtained in step (1) is added in reactor carries out polymerisation, after completion of the reaction
Discharge and the pelletizing after tank cooling；
Step (3)：Dried and solid-phase tack producing after obtained pelletizing in step (2) is extracted；
Step (4)：Finished product is cut into slices.
On this basis, mixed liquor obtained in the step (1) also includes string lysate, is planted in the mixed liquor
The weight portion of fibres lysate is 10~20, and the weight portion of the auxiliary agent is 5~10, the weight portion of the caprolactam solution
It is 70~85.
On this basis, the preparation of the string lysate：By string that weight portion is 90~100 and weight
Part mixes for 2~10 dimethyl sulfoxide, and 2~3 hours are stood after stirring.
On this basis, the string includes seed fiber, leaf fibre and fasciated fiber, and the seed fiber, leaf are fine
The weight ratio of peacekeeping fasciated fiber is 1:1:1.
On this basis, the seed fiber is bombax cotton, and the leaf fibre is abaca fibre, and the fasciated fiber is Asia
Flaxen fiber.
On this basis, the auxiliary agent in the step (1) includes delustering agent, initiator and uvioresistant solvent, described to disappear
The weight ratio of photo etching, initiator and uvioresistant solvent is：2:2:1.
On this basis, the uvioresistant solvent include zinc oxide, and/or titanium dioxide, and/or mineral matter powder and/
Or pearl powder.
On this basis, polymerisation in the step (2) is concretely comprised the following steps：Nitrogen charging displacement is empty in a kettle.
Gas, and the temperature in reactor is heated to 200~250 °, mixed liquor reacts 5~10 hours in a kettle..
On this basis, step (3) concretely comprise the following steps：The pelletizing that step (2) is obtained boiling water extraction 20~
Dried pelletizing is carried out by solid-phase tack producing when 100~120 DEG C of drying 5~10 by drying box after 30 hours.
On this basis, the relative viscosity after the pelletizing solid-phase tack producing in the step (3) is 3.5 ± 0.05.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, a kind of preparation method of the civilian section of level dyeing polyamide fibre 6 that the present invention is provided, comprises the following steps：Will be solid
Intimate lactams is mixed and stirred for uniformly after external heater is melted with auxiliary agent；Mixing liquid obtained in step (1) is added
Entering in reactor carries out polymerisation, after completion of the reaction discharge and the pelletizing after tank cooling；Cut obtained in step (2)
Grain is dried and solid-phase tack producing after being extracted；Finished product is cut into slices.The preparation method of the civilian section of polyamide fibre provided by the present invention 6 is simple
Easily realize, and material good penetrability is spun using the chinlon 6 section is obtained, even dyeing, color fastness is high.
2nd, mixed liquor obtained in the step (1) in the present invention also includes string lysate, and the string includes planting
The weight ratio of subbundle, leaf fibre and fasciated fiber, wherein seed fiber, leaf fibre and fasciated fiber is 1:1:1.In the present invention
String lysate is added with, the permeability of the spinning material of chinlon 6 section production can be effectively improved so that spin material and be more easy to dye
Color.
3rd, the auxiliary agent increase in the step (1) in the present invention has uvioresistant solvent, and the uvioresistant solvent includes oxidation
Zinc, and/or titanium dioxide, and/or mineral matter powder, and/or pearl powder.The uvioresistant solvent can effectively improve polyamide fibre 6 and cut
Piece anti-uv-ray in itself, further increases polyamide fibre 6 and the color fastness for spinning material is obtained.
Brief description of the drawings
Fig. 1 is a kind of schematic flow sheet of the preparation method of the civilian section of level dyeing polyamide fibre 6.
Specific embodiment
Below in conjunction with drawings and Examples, the present invention will be described in further detail.It should be appreciated that described herein
Specific embodiment is only used to explain the present invention, is not intended to limit the present invention.
The present invention discloses a kind of preparation method of the civilian section of level dyeing polyamide fibre 6, as shown in figure 1, including following
Step：
Step (1)：Solid caprolactam is mixed and stirred for uniformly after external heater is melted with auxiliary agent；It is preferred that
Ground, also including string lysate, the weight portion of string lysate is 10~20 in the mixed liquor, the auxiliary agent
Weight portion is 5~10, and the weight portion of the caprolactam solution is 70~85.The wherein preparation of string lysate：Will weight
The dimethyl sulfoxide that amount part is 90~100 string and weight portion is 2~10 mixes, and 2~3 hours are stood after stirring,
String is allowed fully to be reacted with dimethyl sulfoxide so that string is completely dissolved.And it is mixed and made into brocade with other mixing liquids
Synthetic fibre 6, when spinning material is prepared using the polyamide fibre 6, string lysate meets water reuse (treatment, substantially increases the permeability for spinning material.Institute
Stating string includes seed fiber, leaf fibre and fasciated fiber, the weight ratio of the seed fiber, leaf fibre and fasciated fiber
It is 1:1:1.Wherein seed fiber includes cotton fiber, bombax cotton etc., and leaf fibre includes sisal fiber, abaca fibre etc., and stem is fine
Tie up including ramee, flax fiber, flax fiber and tossa etc., it is further preferred that the seed fiber in the present invention
It is bombax cotton, the leaf fibre is abaca fibre, the fasciated fiber is flax fiber.String is added with the present invention molten
Solution liquid, can effectively improve the permeability of the spinning material of chinlon 6 section production so that spin material more easy dyeing.Step in the present invention
(1) auxiliary agent in includes delustering agent, initiator and uvioresistant solvent, the delustering agent, initiator and uvioresistant solvent
Weight ratio is：2:2:1.Preferably, delustering agent is pure PET delustrant RB3329, and initiator is benzoyl peroxide, this
Uvioresistant solvent in invention is included in zinc oxide, and/or titanium dioxide, and/or mineral matter powder, and/or pearl powder at least
Two kinds.The uvioresistant solvent can effectively improve chinlon 6 section anti-uv-ray in itself, further increase polyamide fibre 6
The color fastness for spinning material is obtained.
Step (2)：Mixing liquid obtained in step (1) is added in reactor carries out polymerisation, after completion of the reaction
Discharge and the pelletizing after tank cooling；Wherein polymerisation is concretely comprised the following steps：Nitrogen charging displaced air, and general in a kettle. is instead
The temperature in kettle is answered to be heated to 200~250 °, mixed liquor reacts 5~10 hours in a kettle..
Step (3)：Dried and solid-phase tack producing after obtained pelletizing in step (2) is extracted；Concretely comprise the following steps：Will step
Suddenly the pelletizing that (2) obtain passes through drying box when 100~120 DEG C of drying 5~10, by drying after being extracted 20~30 hours with boiling water
Pelletizing afterwards carries out solid-phase tack producing, and the relative viscosity after gained pelletizing solid-phase tack producing is 3.5 ± 0.05.The specific work of solid-phase tack producing
Skill is：1st, heat up and prepare：Pelletizing is put into the situation of rotary drum sealing, and circulates oil temperature less than 50 DEG C, it is right after sealing rotary drum
Rotary drum carries out positive pressure leak detection and makes corresponding leak source treatment, and carries out examination vacuum to rotary drum.All reached in two premises for heating up
To after technological requirement, can heat up, if there is the condition must not up to heat up.2nd, heat up：The heating schedule includes multiple stages：
2.1st, first stage intensification：Rotating speed 30%, inlet oil temperature enters oil temperature and at the uniform velocity raises 30 DEG C per hour from 100 DEG C, is heated up with this
Then oil-feed temperature rise to 180 DEG C is kept 180 DEG C of inlet oil temperature, until scene temperature rises to 120 DEG C by speed；2.2nd, second-order
Duan Shengwen：After scene temperature reaches 120 DEG C, rotating speed is improved to 40%, by inlet oil temperature with 10 DEG C per hour from 180 DEG C
Heating rate at the uniform velocity rise to 210 DEG C；Enter after oil temperature reaches 210 DEG C, rotating speed is improved to 50%, and with 3 DEG C per hour of intensification
Speed is by oil-feed temperature rise to 240 DEG C；Enter after oil temperature reaches 240 DEG C, rotating speed is improved to 60%, and with 5 DEG C per hour of intensification speed
Rate is by oil-feed temperature rise to 255 DEG C；3rd, it is incubated：Oil-feed temperature rise is to after 255 DEG C, starting insulation.Scene temperature starts after reaching 235 DEG C
Sampling and testing viscosity, took a sample, until reaching viscosity requirement at interval of 1 hour.
Step (4)：Finished product is cut into slices.
Embodiment 1：
A kind of preparation method of the civilian section of level dyeing polyamide fibre 6, comprises the following steps：
Step (1)：Solid caprolactam is mixed after external heater is melted with string lysate and auxiliary agent
And stir；The weight portion of string lysate is 10 in the mixed liquor, and the weight portion of the auxiliary agent is 5, described in oneself
The weight portion of amide solution is 85.The wherein preparation of string lysate：By string and weight portion that weight portion is 90
Dimethyl sulfoxide for 10 mixes, and 3 hours are stood after stirring.Institute's string includes bombax cotton, abaca fibre and flax
Fiber, and the weight ratio of bombax cotton, abaca fibre and flax fiber is 1:1:1.Auxiliary agent include delustering agent, initiator and
Uvioresistant solvent, the weight ratio of the delustering agent, initiator and uvioresistant solvent is：2:2:1.Wherein uvioresistant
Solvent is zinc oxide and titanium dioxide mixed solution, and the weight ratio of zinc oxide and carbon dioxide is 1：1.
Step (2)：Mixing liquid obtained in step (1) is added in reactor carries out polymerisation, after completion of the reaction
Discharge and the pelletizing after tank cooling；Wherein polymerisation is concretely comprised the following steps：Nitrogen charging displaced air, and general in a kettle. is instead
The temperature in kettle is answered to be heated to 200 °, mixed liquor reacts 10 hours in a kettle..
Step (3)：Dried and solid-phase tack producing after obtained pelletizing in step (2) is extracted；Concretely comprise the following steps：Will step
Suddenly the pelletizing that (2) obtain passes through drying box when 120 DEG C of dryings 5 after being extracted 20 hours with boiling water, dried pelletizing is carried out
Solid-phase tack producing, the relative viscosity after gained pelletizing solid-phase tack producing is 3.55.
Step (4)：Finished product is cut into slices.
Embodiment 2：
A kind of preparation method of the civilian section of level dyeing polyamide fibre 6, comprises the following steps：
Step (1)：Solid caprolactam is mixed after external heater is melted with string lysate and auxiliary agent
And stir；The weight portion of string lysate is 12 in the mixed liquor, and the weight portion of the auxiliary agent is 7, described in oneself
The weight portion of amide solution is 71.The wherein preparation of string lysate：By string and weight portion that weight portion is 95
Dimethyl sulfoxide for 5 mixes, and 2 hours are stood after stirring.Institute's string includes that bombax cotton, abaca fibre and flax are fine
Dimension, and the weight ratio of bombax cotton, abaca fibre and flax fiber is 1:1:1.Auxiliary agent includes delustering agent, initiator and resists
Ultraviolet solvent, the weight ratio of the delustering agent, initiator and uvioresistant solvent is：2:2:1.Wherein uvioresistant is molten
Agent is the mixed solution for including zinc oxide and mineral matter powder, and the weight ratio of zinc oxide and mineral matter powder is 2:1.
Step (2)：Mixing liquid obtained in step (1) is added in reactor carries out polymerisation, after completion of the reaction
Discharge and the pelletizing after tank cooling；Wherein polymerisation is concretely comprised the following steps：Nitrogen charging displaced air, and general in a kettle. is instead
The temperature in kettle is answered to be heated to 220 °, mixed liquor reacts 7 hours in a kettle..
Step (3)：Dried and solid-phase tack producing after obtained pelletizing in step (2) is extracted；Concretely comprise the following steps：Will step
Suddenly the pelletizing that (2) obtain passes through drying box when 115 DEG C of dryings 5 after being extracted 22 hours with boiling water, dried pelletizing is carried out
Solid-phase tack producing, the relative viscosity after gained pelletizing solid-phase tack producing is 3.55.
Step (4)：Finished product is cut into slices.
Embodiment 3：
A kind of preparation method of the civilian section of level dyeing polyamide fibre 6, comprises the following steps：
Step (1)：Solid caprolactam is mixed after external heater is melted with string lysate and auxiliary agent
And stir；The weight portion of string lysate is 16 in the mixed liquor, and the weight portion of the auxiliary agent is 8, described in oneself
The weight portion of amide solution is 76.The wherein preparation of string lysate：By string and weight portion that weight portion is 96
Dimethyl sulfoxide for 4 mixes, and 2.5 hours are stood after stirring.Institute's string includes bombax cotton, abaca fibre and flax
Fiber, and the weight ratio of bombax cotton, abaca fibre and flax fiber is 1:1:1.Auxiliary agent include delustering agent, initiator and
Uvioresistant solvent, the weight ratio of the delustering agent, initiator and uvioresistant solvent is：2:2:1.Wherein uvioresistant
The mixed solution of solvent including zinc oxide, mineral matter powder and pearl powder, and zinc oxide, mineral matter powder and pearl powder weight portion it
Than being 1.5:1:0.8.
Step (2)：Mixing liquid obtained in step (1) is added in reactor carries out polymerisation, after completion of the reaction
Discharge and the pelletizing after tank cooling；Wherein polymerisation is concretely comprised the following steps：Nitrogen charging displaced air, and general in a kettle. is instead
The temperature in kettle is answered to be heated to 230 °, mixed liquor reacts 5.5 hours in a kettle..
Step (3)：Dried and solid-phase tack producing after obtained pelletizing in step (2) is extracted；Concretely comprise the following steps：Will step
Suddenly the pelletizing that (2) obtain passes through drying box when 126 DEG C of dryings 5 after being extracted 23 hours with boiling water, dried pelletizing is carried out
Solid-phase tack producing, the relative viscosity after gained pelletizing solid-phase tack producing is 3.55.
Step (4)：Finished product is cut into slices.
Embodiment 4：
A kind of preparation method of the civilian section of level dyeing polyamide fibre 6, comprises the following steps：
Step (1)：Solid caprolactam is mixed after external heater is melted with string lysate and auxiliary agent
And stir；The weight portion of string lysate is 18 in the mixed liquor, and the weight portion of the auxiliary agent is 8, described in oneself
The weight portion of amide solution is 74.The wherein preparation of string lysate：By string and weight portion that weight portion is 96
Dimethyl sulfoxide for 7.5 mixes, and 2.5 hours are stood after stirring.Institute's string includes bombax cotton, abaca fibre and Asia
Flaxen fiber, and the weight ratio of bombax cotton, abaca fibre and flax fiber is 1:1:1.Auxiliary agent includes delustering agent, initiator
With uvioresistant solvent, the weight ratio of the delustering agent, initiator and uvioresistant solvent is：2:2:1.Wherein uvioresistant
The mixed solution of line solvent including zinc oxide, titanium dioxide and pearl powder, and zinc oxide, titanium dioxide and pearl powder weight portion
The ratio between be 2:2:1.
Step (2)：Mixing liquid obtained in step (1) is added in reactor carries out polymerisation, after completion of the reaction
Discharge and the pelletizing after tank cooling；Wherein polymerisation is concretely comprised the following steps：Nitrogen charging displaced air, and general in a kettle. is instead
The temperature in kettle is answered to be heated to 235 °, mixed liquor reacts 7 hours in a kettle..
Step (3)：Dried and solid-phase tack producing after obtained pelletizing in step (2) is extracted；Concretely comprise the following steps：Will step
Suddenly the pelletizing that (2) obtain passes through drying box when 110 DEG C of dryings 5 after being extracted 25 hours with boiling water, dried pelletizing is carried out
Solid-phase tack producing, the relative viscosity after gained pelletizing solid-phase tack producing is 3.55.
Step (4)：Finished product is cut into slices.
Embodiment 5：
A kind of preparation method of the civilian section of level dyeing polyamide fibre 6, comprises the following steps：
Step (1)：Solid caprolactam is mixed after external heater is melted with string lysate and auxiliary agent
And stir；The weight portion of string lysate is 20 in the mixed liquor, and the weight portion of the auxiliary agent is 10, described in oneself
The weight portion of amide solution is 70.The wherein preparation of string lysate：By string and weight portion that weight portion is 98
Dimethyl sulfoxide for 2 mixes, and 3 hours are stood after stirring.Institute's string includes that bombax cotton, abaca fibre and flax are fine
Dimension, and the weight ratio of bombax cotton, abaca fibre and flax fiber is 1:1:1.Auxiliary agent includes delustering agent, initiator and resists
Ultraviolet solvent, the weight ratio of the delustering agent, initiator and uvioresistant solvent is：2:2:1.Wherein uvioresistant is molten
Agent includes the mixed solution of titanium dioxide and/or mineral matter powder, and the weight ratio of titanium dioxide and/or mineral matter powder is 3:1.
Step (2)：Mixing liquid obtained in step (1) is added in reactor carries out polymerisation, after completion of the reaction
Discharge and the pelletizing after tank cooling；Wherein polymerisation is concretely comprised the following steps：Nitrogen charging displaced air, and general in a kettle. is instead
The temperature in kettle is answered to be heated to 250 °, mixed liquor reacts 8 hours in a kettle..
Step (3)：Dried and solid-phase tack producing after obtained pelletizing in step (2) is extracted；Concretely comprise the following steps：Will step
Suddenly the pelletizing that (2) obtain passes through drying box when 110 DEG C of dryings 6 after being extracted 28 hours with boiling water, dried pelletizing is carried out
Solid-phase tack producing, the relative viscosity after gained pelletizing solid-phase tack producing is 3.55.
Step (4)：Finished product is cut into slices.
Experimental comparison：
Chinlon 6 section and common sample obtained by embodiment 1~5 is carried out into Experimental comparison, 1, production equal number
Chinlon 6 section, because dyeing is uneven, probability that is producing substandard products is 25% in common sample production process, and embodiment 1~5
Obtained chinlon 6 section is below 5% due to dyeing the uneven two substandard products probability for producing, and the probability of embodiment 5 is minimum.
2nd, in the environment of being 52% in relative humidity, to the chinlon 6 section obtained by common sample and embodiment 1~5, it is with optical wavelength
The light source of 300nm is irradiated, and the duration is 480 hours, and to each sample carries out colourity collection and contrast every three days.
Can be obtained by experiment, common sample before 120 hours, the color fastness of common sample reduction by 25%, and the gained sample of embodiment 1~5
It is held in more than 95%.After 480 hours, the color fastness of embodiment 1,2 and 5 is kept at 90% or so, embodiment 3 and 4
More than 92%, by data above as can be seen that the gained sample even dyeing of embodiment 1~5, final product quality is high for color fastness, and
Aging speed is slower, and color fastness to light is high, solves the problems, such as that polyamide fibre macromolecular is fast light and heat-resistant stability is poor.
Described above has shown and described the preferred embodiments of the present invention, as previously described, it should be understood that not office of the invention
Be limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and can be used for various other combinations, modification and
Environment, and can be changed by the technology or knowledge of above-mentioned teaching or association area in invention contemplated scope described herein
It is dynamic.And the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention, then all should be appended by the present invention
In scope of the claims.
Claims (10)
1. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6, it is characterised in that：Comprise the following steps：
Step (1)：Solid caprolactam is mixed and stirred for uniformly after external heater is melted with auxiliary agent；
Step (2)：Mixing liquid obtained in step (1) is added in reactor carries out polymerisation, after completion of the reaction discharge
And pelletizing after being cooled down through tank；
Step (3)：Dried and solid-phase tack producing after obtained pelletizing in step (2) is extracted；
Step (4)：Finished product is cut into slices.
2. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 1, it is characterised in that：Institute
Stating mixed liquor obtained in step (1) also includes string lysate, the weight portion of string lysate in the mixed liquor
It is 10~20, the weight portion of the auxiliary agent is 5~10, the weight portion of the caprolactam solution is 70~85.
3. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 2, it is characterised in that：Institute
State the preparation of string lysate：The string that weight portion is 90~100 and the dimethyl sulfoxide that weight portion is 2~10 are mixed
Close, 2~3 hours are stood after stirring.
4. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 3, it is characterised in that：Institute
Stating string includes seed fiber, leaf fibre and fasciated fiber, the weight ratio of the seed fiber, leaf fibre and fasciated fiber
It is 1:1:1.
5. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 4, it is characterised in that：Institute
Seed fiber is stated for bombax cotton, the leaf fibre is abaca fibre, the fasciated fiber is flax fiber.
6. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 1, it is characterised in that：Institute
The auxiliary agent stated in step (1) includes delustering agent, initiator and uvioresistant solvent, the delustering agent, initiator and uvioresistant
The weight ratio of solvent is：2:2:1.
7. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 6, it is characterised in that：Institute
Stating uvioresistant solvent includes zinc oxide, and/or titanium dioxide, and/or mineral matter powder, and/or pearl powder.
8. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 1, it is characterised in that：Institute
State concretely comprising the following steps for the polymerisation in step (2)：Nitrogen charging displaced air in a kettle., and the temperature in reactor is added
To 200~250 °, mixed liquor reacts 5~10 hours to heat in a kettle..
9. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 1, it is characterised in that：Institute
State concretely comprising the following steps for step (3)：The pelletizing that step (2) is obtained with boiling water extract 20~30 hours after by drying box in
During 100~120 DEG C of drying 5~10, dried pelletizing is carried out into solid-phase tack producing.
10. the preparation method of the civilian section of a kind of level dyeing polyamide fibre 6 according to claim 9, it is characterised in that：Institute
It is 3.5 ± 0.05 to state the relative viscosity after the pelletizing solid-phase tack producing in step (3).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710007964.2A CN106674515A (en) | 2017-01-05 | 2017-01-05 | Method for preparing nylon 6 civil chips with uniform dyeing properties |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710007964.2A CN106674515A (en) | 2017-01-05 | 2017-01-05 | Method for preparing nylon 6 civil chips with uniform dyeing properties |
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| CN201710007964.2A Pending CN106674515A (en) | 2017-01-05 | 2017-01-05 | Method for preparing nylon 6 civil chips with uniform dyeing properties |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885842A (en) * | 2010-07-09 | 2010-11-17 | 北京三联虹普纺织化工技术有限公司 | Continuous polymerization production technology for polyamide fibre 6 |
| CN102337026A (en) * | 2010-07-22 | 2012-02-01 | 合肥杰事杰新材料股份有限公司 | Preparation method of natural plant cellulose-modified PA6 composite material |
| CN103044911A (en) * | 2012-12-21 | 2013-04-17 | 湖北工业大学 | Nylon 6/plant fiber composite material and preparation method thereof |
| CN103421184A (en) * | 2013-08-05 | 2013-12-04 | 福建景丰科技有限公司 | Method for preparing chinlon 6 slices |
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2017
- 2017-01-05 CN CN201710007964.2A patent/CN106674515A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885842A (en) * | 2010-07-09 | 2010-11-17 | 北京三联虹普纺织化工技术有限公司 | Continuous polymerization production technology for polyamide fibre 6 |
| CN102337026A (en) * | 2010-07-22 | 2012-02-01 | 合肥杰事杰新材料股份有限公司 | Preparation method of natural plant cellulose-modified PA6 composite material |
| CN103044911A (en) * | 2012-12-21 | 2013-04-17 | 湖北工业大学 | Nylon 6/plant fiber composite material and preparation method thereof |
| CN103421184A (en) * | 2013-08-05 | 2013-12-04 | 福建景丰科技有限公司 | Method for preparing chinlon 6 slices |
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