CN104878618A - Method for dyeing superfine terylene fabric - Google Patents

Method for dyeing superfine terylene fabric Download PDF

Info

Publication number
CN104878618A
CN104878618A CN201510266835.6A CN201510266835A CN104878618A CN 104878618 A CN104878618 A CN 104878618A CN 201510266835 A CN201510266835 A CN 201510266835A CN 104878618 A CN104878618 A CN 104878618A
Authority
CN
China
Prior art keywords
dyeing
dye
ultra
agent
polyester fabric
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201510266835.6A
Other languages
Chinese (zh)
Other versions
CN104878618B (en
Inventor
张贵
张烨
王思捷
皮建兵
张新华
李明辉
刘珊
黄至薪
陈臻
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hutai Panyu Textile and Dyeing Co Ltd
Original Assignee
Hutai Panyu Textile and Dyeing Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hutai Panyu Textile and Dyeing Co Ltd filed Critical Hutai Panyu Textile and Dyeing Co Ltd
Priority to CN201510266835.6A priority Critical patent/CN104878618B/en
Publication of CN104878618A publication Critical patent/CN104878618A/en
Application granted granted Critical
Publication of CN104878618B publication Critical patent/CN104878618B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Coloring (AREA)

Abstract

The invention discloses a method for dyeing a superfine terylene fabric. The method comprises the following dyeing steps: adding a softening agent, part of a leveling agent, and an expansive agent into the soppy superfine terylene fabric to prepare a working solution; adding a pH regulator to regulate the pH value of the working solution to 3.5-4.0; heating the working solution with the adjusted pH value to 43 DEG C, and adding disperse dye and the residual leveling agent to prepare a dye liquor; carrying out heating and dyeing. The method aims at dyeing of a brightly colored superfine terylene fabric, and has the advantages the softening agent, the leveling agent and the expansive agent are added simultaneously, and the pH value of the dye liquor is regulated to 3.5-4.0, so that poor leveling property, uneven dyeing and other quality problems existing in a low-bath-ratio dyeing process can be solved; moreover, the dye-uptake rate of the disperse dye can be improved, secondary aggregation of the disperse dye in a high-temperature descending process is prevented, all color fastness indices of the superfine terylene fabric exceed 4-level, the dyeing property is improved, and the dyeing effect is ideal; the method further has the advantages of being environment-friendly and low in energy consumption.

Description

A kind of colouring method of Polyester Fabric of Ultra-fine Fibre under Alkali Condition
Technical field
The invention belongs to technical field of textile printing, be specifically related to a kind of colouring method of Polyester Fabric of Ultra-fine Fibre under Alkali Condition.
Background technology
Ultra-fine polyester fiber has good, the ventilative moisture absorption of soft, slim and graceful drapability, the excellent properties such as comfortable and easy to wear.At present, Polyester Fabric of Ultra-fine Fibre under Alkali Condition dyeing mainly contains high-temperature and high pressure dyeing process, and thermosol dyeing method and carrier dyeing process, wherein high-temperature and high pressure dyeing process is the most conventional.During super fine polyester high-temperature pressure dyeing, should numerator value be selected minimum, the low form dyestuff that dispersive property is good as far as possible.
In recent years, some bright-coloured, beautiful colors such as color orchid, gorgeous blue look become main flow, and dyeing adopts the color blue SWF molecular mass super large of DISPERSE DYES, and intermolecular force is strong.In dyeing and finishing process technology, face level-dyeing property difference, look flower, particularly more easily occur the quality problem such as look flower, color dot, Duan Hua in the dyeing of low bath raio air-flow cylinder, face and be difficult to repair look.
Chinese patent CN102628211B discloses Polyester Fabric of Ultra-fine Fibre under Alkali Condition dyeing and finishing processing method, comprises following procedure of processing: (1) pre-treatment: cold-pad-batch process processing terylene grey fabric being comprised to cold dome, hot alkali treatment and efficient washing three phases; (2) pre-setting: setting machine high temperature tentering pre-setting is used to the fabric openpore after pre-treatment; (3) dye: adopt superfine fibre levelling agent to dye to the fabric openpore after pre-setting; (4) clean: cleaning post processing is carried out to fabric after dyeing, the DISPERSE DYES of non-set after removal stock-dye.The novel dyeing and finishing processing technology of this invention adopts environmental protection, the cold-pad-batch preparation technology of low energy consumption carries out pre-treatment to Polyester Fabric of Ultra-fine Fibre under Alkali Condition, and destarch is effective on the one hand, for dyeing provides good dyeing and finishing processing conditions, on the other hand, effectively can reduce fabric wrinkle print.But the Polyester Fabric of Ultra-fine Fibre under Alkali Condition dyeing and finishing processing method of this invention is not suitable for the dyeing of bright-colored, beautiful Polyester Fabric of Ultra-fine Fibre under Alkali Condition, the quality problem such as level-dyeing property difference, look flower is there is in dyeing and finishing process technology, especially when low bath raio, more easily there is the quality problem such as look flower, color dot, Duan Hua, and be difficult to repair look.
Summary of the invention
The object of the present invention is to provide a kind of colouring method of Polyester Fabric of Ultra-fine Fibre under Alkali Condition, the level-dyeing property that brightly painted Polyester Fabric of Ultra-fine Fibre under Alkali Condition exists in low bath raio dyeing and finishing process technology be poor to solve, the quality problem such as look flower.
For reaching this object, the present invention by the following technical solutions:
A kind of colouring method of Polyester Fabric of Ultra-fine Fibre under Alkali Condition, comprise staining procedure: in the Polyester Fabric of Ultra-fine Fibre under Alkali Condition soaked, add softener, part levelling agent and swelling agent be made into working solution, and add pH adjusting agent adjustment working solution pH to 3.5 ~ 4.0, add DISPERSE DYES when being warming up to 43 DEG C and remain levelling agent and be made into dye liquor, then heat up dyeing.For the colouring method of Polyester Fabric of Ultra-fine Fibre under Alkali Condition, the colouring method of especially brightly painted Polyester Fabric of Ultra-fine Fibre under Alkali Condition, is adjusted to the quality problem such as the level-dyeing property existed when can solve low bath ratio dyeing after 3.5 ~ 4.0 is poor, look flower by dye liquor pH.
Above-mentioned Polyester Fabric of Ultra-fine Fibre under Alkali Condition adopts and adds water-soaked, and wherein the consumption of water is the capacity of dyeing machine of the present invention.In staining procedure, the mixing of water, other auxiliary agents of dye well is dye liquor of the present invention." g/L " in following staining procedure all refers to the quality (gram) of the material that every premium on currency adds.
DISPERSE DYES of the present invention, is specially decentralized high temperature modification dyestuff, has higher sublimation reliability.But because molecular structure is more complicated, affinity is higher, the diffusion rate in polyster fibre is comparatively slow, and uniform dyeing property is poor, often occurs the quality problem such as color dot, look flower.It is blue that described DISPERSE DYES comprises Foron CYANINESWF, and other DISPERSE DYES can also be selected combined with it, and such as MEKICRON VIOLET FBL is blue, MEKICRON BLUE BG is blue.
Described Polyester Fabric of Ultra-fine Fibre under Alkali Condition dyes in airflow dyeing machine, and dye bath ratio is 1:4 ~ 8, such as 1:4,1:5,1:6,1:7,1:8.Airflow dyeing machine is adopted to dye to Polyester Fabric of Ultra-fine Fibre under Alkali Condition under low bath raio condition, energy-conserving and environment-protective.
The heating rate that described working solution is warming up to 43 DEG C is 3 DEG C/min; Described intensification dyeing adopts sectional type to heat up: control dye liquor with the ramp to 100 DEG C of 2 DEG C/min, then with the ramp to 110 DEG C of 0.8 DEG C/min, finally with DEG C insulation of the ramp to 130 of 1.8 DEG C/min, sectional type dyeing heating process flow process is shown in Fig. 1, and the dyestuff wherein in accompanying drawing 1 refers to DISPERSE DYES.Control intensification decoration method be from begin dye temperature to dye balance temperature contaminate characteristic by dyestuff and strictly control heating rate, intensifications of slowing down in the temperature range that dye-uptake is high, even at this temperature dyeing certain hour, and then continue to heat up and dye.Adopt sectional type temperature-rising method of the present invention that DISPERSE DYES can be made to keep dye-uptake more slowly, thus it is more even that Polyester Fabric of Ultra-fine Fibre under Alkali Condition is dyeed.
Dye liquor linearly adds DISPERSE DYES and residue levelling agent again when being warming up to 43 DEG C, the linear joining day of the DISPERSE DYES added when described 43 DEG C and residue levelling agent is 20min; Described levelling agent is PRDN, described part levelling agent is 0.5 ~ 4g/L with the consumption sum of residue levelling agent, such as 0.6g/L, 0.65g/L, 0.7g/L, 0.8g/L, 0.9g/L, 1g/L, 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, described part levelling agent is 2:1 with the mass ratio of residue levelling agent.Levelling agent PRDN first adds 2/3 before dye liquor heats up, and linearly adds levelling agent again, effectively can reduce the gathering of dyestuff when being warming up to 43 DEG C of insulations.
The consumption of described DISPERSE DYES is 0.6 ~ 6% (OWF), such as 0.7% (OWF), 0.8% (OWF), 0.9% (OWF), 1% (OWF), 1.1% (OWF), 1.2% (OWF), 1.3% (OWF), 1.5% (OWF), 1.8% (OWF), 2% (OWF), 2.2% (OWF), 2.4% (OWF), 2.5% (OWF), 2.8% (OWF), 3% (OWF), 3.2% (OWF), 3.4% (OWF), 3.5% (OWF), 3.7% (OWF), 3.8% (OWF), 3.9% (OWF), 4% (OWF), 4.2% (OWF), 4.5% (OWF), 5% (OWF), 5.5% (OWF), 6% (OWF).
Because super fine polyester specific surface is knitted greatly, low bath ratio dyeing raises with temperature, easily occurs that upper dye is too fast, produces look flower, a difference, and the molecular weight ratio of DISPERSE DYES is comparatively large, especially disperses gorgeous blue SWF molecular weight super large, easily assembles in dyeing course.Produce heat-aggregated reason mainly along with the raising of temperature; the activation energy of dyestuff self increases thereupon; the probability that dyestuff crystal grain collides increases; the dyestuff micelle that those dispersion stabilizations are poor or free dyestuff crystal grain just can reassemble; form new or larger dye granule, so dye aggregation body.In high temperature temperature-fall period, dyestuff also can because of the reduction of water temperature, and thermal vibration weakens, and solubility declines, and dyestuff is separated out and secondary aggregation occurs.This " heat-aggregated " of DISPERSE DYES, has generally believed three kinds of situations:
(1) the dyestuff unimolecule dissolved is adsorbed on again dye crystal surface, and crystal grain is increased, and its crystal formation is constant.
(2) free dye molecule or crystal grain are assembled again, form new crystal formation.
(3) small dyestuff crystal grain is without the dye granule dissolved, direct collision formation is larger, and this phenomenon usually occurs in the temperature rise period.This large dye aggregation body not only affects level dyeing, thoroughly contaminates effect, even can produce " tar compound " and cause the dye defect that cannot repair.Fig. 3 is shown in by the high temperature aggregation schematic diagram of DISPERSE DYES.
Described softener is CN, and the consumption of described softener is 1 ~ 3g/L, such as 1.2g/L, 1.3g/L, 1.5g/L, 1.4g/L, 1.5g/L, 1.8g/L, 2g/L, 2.2g/L, 2.5g/L, 2.8g/L.Softener CN of the present invention is wetting softener, and the effect of wetting softener is the friction factor reducing fabric and equipment, thus reduces the generation of fabric scratch and wrinkle trace.
Described swelling agent is DFM, and the consumption of described swelling agent is 0.5 ~ 2g/L; Disperse the molecular mass of gorgeous blue SWF or other large molecule DISPERSE DYES very large, even if polyster fibre more difficult to get access is inner below for DEG C dyeing condition in high temperature of 120 DEG C ~ 130, diffusion rate in polyster fibre is also slow, longer high-temperature holding time must be had, add swelling agent DFM can effectively to expand the intermolecular space of super fine polyester, the gorgeous blue SWF supramolecular of dispersion can better be spread in super fine polyester, and also evenly dye reappearance is effective thoroughly can to reach dye balance faster.
PH value is little on conventional DISPERSE DYES impact, as long as even if pH value controls some fluctuation in 3 ~ 6 scopes, also very little on the impact of dye-uptake, can not cause obvious aberration.Under the condition of pH > 6, can there is hydrolysis in conventional DISPERSE DYES, and look can shoal, coloured light mutation.But for the gorgeous blue SWF of DISPERSE DYES, in actual production, between traditional HAc and NaAc cushioning liquid control pH=4.5 ~ 5, during dyeing, Dry Sack rate is low, easily occurs color dot.Therefore the present invention adopts citric acid as pH adjusting agent, and the consumption of described citric acid is 0.5 ~ 1g/L.Adopt traditional HAc/NaAc cushioning liquid also can regulate the pH of dye liquor, but when pH is adjusted to 3.5 ~ 4, the consumption of HAc is a lot, easy volatilization, contaminated environment, and adopt citric acid to regulate dye liquor pH, can avoid selecting traditional HAc/NaAc cushioning liquid to regulate the HAc occurred during dye liquor pH to hold volatile problem, low bath ratio dyeing also makes colouring method of the present invention also have the advantage of Environmentally-frielow-energy-consumptipolycarboxylic low-energy-consumptipolycarboxylic.
The time of described 130 DEG C of insulations is 30min.
Also need to lower the temperature after described intensification dyeing, described cooling is sectional type cooling: after control dye liquor is cooled to 110 DEG C with 4 DEG C/min, is cooled to 95 DEG C, is finally cooled to 70 DEG C of drainings with 1.5 DEG C/min with 2.5 DEG C/min.
High Temperature Pre fixating shape step is also comprised: Polyester Fabric of Ultra-fine Fibre under Alkali Condition is placed in pre-setting machine, pre-setting process 20 ~ 30s under 190 DEG C of conditions before described staining procedure.Super fine polyester stockinette is easy contraction distortion under damp and hot hot conditions, fabric is made to produce permanent wrinkle print, be difficult to eliminate, High Temperature Pre sizing can reduce or eliminate super fine polyester stockinette at spinning drawing with to weave the tension force produced in processing irregular, while can avoid super fine polyester stockinette overrelaxation and crimping generation dyeing flower.But too the predetermined grey cloth of high-temperature can cause the loss of fabric elastic, conservative control preboarding condition should be required according to fabric specification and finished product elastic force.
Also reduction clearing step is comprised: add water and NaOH is made into cleaning fluid after described staining procedure, cleaning fluid takes a policy after being warming up to 60 DEG C powder process, then the cleaning fluid controlled after sodium hydrosulfite process is warming up to 85 DEG C of insulations, be cooled to 70 DEG C of drainings again, finally neutralisation treatment carried out to the Polyester Fabric of Ultra-fine Fibre under Alkali Condition after reduction cleaning.Fig. 2 is shown in the technological process of reduction cleaning.
The consumption of the water in reduction clearing step of the present invention is the capacity of airflow dyeing machine.Wherein " g/L " all refers to the quality (g) of the material that every premium on currency adds.
The consumption of described NaOH is 4 ~ 6g/L;
The heating rate that described cleaning fluid is warming up to 60 DEG C is 4 DEG C/min;
The heating rate that cleaning fluid after sodium hydrosulfite process is warming up to 85 DEG C is 3 DEG C/min, and temperature retention time is 9min; Described sodium hydrosulfite adds at twice: first add 1/2 sodium hydrosulfite insulation 3min, and then add residue 1/2 sodium hydrosulfite insulation 3min; Sodium hydrosulfite adds the loose colour being conducive to washing Polyester Fabric of Ultra-fine Fibre under Alkali Condition fiber surface further at twice.
The rate of temperature fall that described cleaning fluid is cooled to 70 DEG C is 1.5 DEG C/min;
Described neutralisation treatment comprises: in the Polyester Fabric of Ultra-fine Fibre under Alkali Condition after reduction cleaning, add water and 0.3g/L citric acid, with draining after the ramp to 70 of 3 DEG C/min DEG C cleaning 5min, then adds water and 0.2g/L citric acid, draining after cleaning 5min.Adopt draining again after sour neutralisation treatment, then the alkali lye washed on dacron can also avoid contaminated environment simultaneously.
Compared with prior art, beneficial effect of the present invention is: comprise staining procedure: in the Polyester Fabric of Ultra-fine Fibre under Alkali Condition soaked, add softener, part levelling agent and swelling agent be made into working solution, and add pH adjusting agent adjustment working solution pH to 3.5 ~ 4.0, add DISPERSE DYES when being warming up to 43 DEG C and remain levelling agent and be made into dye liquor, then heat up dyeing.For the colouring method of Polyester Fabric of Ultra-fine Fibre under Alkali Condition, the colouring method of especially brightly painted Polyester Fabric of Ultra-fine Fibre under Alkali Condition, adds softener, levelling agent and swelling agent in dye liquor simultaneously and dye liquor pH is adjusted to the quality problem such as 3.5 ~ 4.0 level-dyeing properties existed when can solve low bath ratio dyeing are poor, look flower.Adopt colouring method of the present invention can improve the dye-uptake of DISPERSE DYES, prevent from, in dyestuff high temperature temperature-fall period, Second Aggregation occurs, and ensure that every COLOR FASTNESS of Polyester Fabric of Ultra-fine Fibre under Alkali Condition reaches more than 4 grades, improve dyeability, obtain desirable Color, also there is the advantage of Environmentally-frielow-energy-consumptipolycarboxylic low-energy-consumptipolycarboxylic simultaneously.
Accompanying drawing explanation
Fig. 1 is the process chart of staining procedure of the present invention.
Fig. 2 is the process chart of reduction clearing step of the present invention.
Fig. 3 is the high temperature aggregation schematic diagram of existing DISPERSE DYES.
Fig. 4 is the dye-uptake that levelling agent PRDN of the present invention disperses gorgeous blue SWF under condition of different temperatures.
Fig. 5 is the dye-uptake that existing leveling agent d PS disperses gorgeous blue SWF under condition of different temperatures.
Fig. 6 is the dye-uptake of the gorgeous blue SWF of dispersion when not adding levelling agent.
Detailed description of the invention
Technical scheme of the present invention is further illustrated by detailed description of the invention below in conjunction with accompanying drawing 1 ~ 6.
As no specific instructions, various raw material of the present invention all can commercially availablely be buied, or prepares according to the conventional method of this area.
Embodiment 1 disperses gorgeous blue Polyester Fabric of Ultra-fine Fibre under Alkali Condition (light color)
Fabric: super fine polyester 500Kg (88%Poly+12%Lycra), specification is 50D/144F SD Poly+40DLycra, door width 160cm, grammes per square metre 95g/m 2
Dyeing machine: THEN airflow dyeing machine
Dyeing recipe is as follows:
Polyester Fabric of Ultra-fine Fibre under Alkali Condition is placed in pre-setting machine, at 190 DEG C of pre-setting process 20s, then Polyester Fabric of Ultra-fine Fibre under Alkali Condition is placed in dyeing machine, add water-soaked, the gorgeous orchid of dispersion is added by above-mentioned formula, softener, 2/3 levelling agent and swelling agent, add lemon acid for adjusting pH to 3.92, with the ramp to 43 DEG C of 3 DEG C/min, and linearly add DISPERSE DYES Foron CYANINE SWF orchid and residue 1/3 levelling agent (joining day is 20min), with the ramp to 100 DEG C of 2 DEG C/min, then 110 DEG C are warming up to 0.8 DEG C/min, 130 DEG C of insulation 30min are warming up to again with 1.3 DEG C/min, finally to lower the temperature process: after being cooled to 110 DEG C with 4 DEG C/min, 95 DEG C are cooled to 2.5 DEG C/min, finally be cooled to 70 DEG C of drainings with 1.5 DEG C/min, add water, 4g/L NaOH, after being warming up to 60 DEG C with 4 DEG C/min, adding 1/2 process 3min of 4g/L sodium hydrosulfite, then add 1/2 remaining sodium hydrosulfite process 3min, be warming up to 85 DEG C of process 9min with 3 DEG C/min, be then cooled to 70 DEG C with 1.7 DEG C/min, draining, add water, 0.3g/L citric acid, with 3 DEG C/min be warming up to 70 DEG C process 5min, draining, add water, 0.2g/L citric acid, cleaning 5min, draining.Carry out post processing again, obtained blue look Polyester Fabric of Ultra-fine Fibre under Alkali Condition (light color).
Embodiment 2 disperses gorgeous blue Polyester Fabric of Ultra-fine Fibre under Alkali Condition (middle look)
Fabric and dyeing machine are all identical with embodiment 1.
Dyeing recipe is as follows:
According to above-mentioned formula and bath raio, adopt the colouring method identical with embodiment 1 to prepare blue look Polyester Fabric of Ultra-fine Fibre under Alkali Condition (middle look), difference is that the time of pre-setting process is 30s, adopts lemon acid for adjusting pH to 3.75.
Embodiment 3 disperses gorgeous blue Polyester Fabric of Ultra-fine Fibre under Alkali Condition (dark color)
Fabric and dyeing machine are all identical with embodiment 1.
Dyeing recipe:
According to above-mentioned formula and bath raio, adopt the colouring method identical with embodiment 1 to prepare blue look Polyester Fabric of Ultra-fine Fibre under Alkali Condition (dark color), difference is to adopt lemon acid for adjusting pH to 3.56, and the addition of NaOH and sodium hydrosulfite is 6g/L.
Embodiment 4
Fabric and dyeing machine are all identical with embodiment 1.
Dyeing recipe:
According to above-mentioned dyeing recipe and bath raio, the colouring method identical with embodiment 1 is adopted to prepare blue look Polyester Fabric of Ultra-fine Fibre under Alkali Condition (middle look).
Embodiment 5
Fabric and dyeing machine are all identical with embodiment 1.
Dyeing recipe:
According to above-mentioned dyeing recipe and bath raio, the colouring method identical with embodiment 1 is adopted to prepare blue look Polyester Fabric of Ultra-fine Fibre under Alkali Condition (dark color).
Comparative example 1
The consumption of citric acid is 0.4g/L, and other are all identical with embodiment 1.
Comparative example 2
The consumption of citric acid is 0.2g/L, and other are all identical with embodiment 1.
Comparative example 3
Not adding citric acid, other are all identical with embodiment 1.
Comparative example 4
Adopt HAc/NaAc buffer solution to regulate dye liquor pH, concrete consumption is in table 2, and other are all identical with embodiment 1.
Comparative example 5
Levelling agent PRDN is disposable before dye liquor heats up to add, and other are all identical with embodiment 1.
The K/S value of the Polyester Fabric of Ultra-fine Fibre under Alkali Condition after dyeing in test above-described embodiment 1 ~ 3, comparative example 1 ~ 3 (adopting citric acid to regulate dyeing pH) and Color are in table 1, and the K/S value of the Polyester Fabric of Ultra-fine Fibre under Alkali Condition after test comparison example 4 dyes (adopting HAc/NaAc cushioning liquid to regulate dyeing pH) and Color are in table 2.
The Color of Polyester Fabric of Ultra-fine Fibre under Alkali Condition after table 1. lemon acid for adjusting pH
The Color of Polyester Fabric of Ultra-fine Fibre under Alkali Condition after table 2.HAc/NaAc cushioning liquid adjustment pH
Found by contrast table 1, table 2, the Color impact of pH value on the gorgeous blue SWF of DISPERSE DYES is comparatively large, and when pH value 3.5 ~ 4.0, fabric K/S value is the highest.Effect is fine, and pH value raises gradually, and K/S value reduces gradually, and color dot is more serious.Illustrate that pH is higher, gorgeous blue SWF dyestuff generation secondary aggregation, produce Shared-with point.PH value should control between 3.5 ~ 4.0, but weak acid HAc is difficult to stable control pH between 3.5 ~ 4.0, and the HAc high volatility of high concentration, smell is very large, easy contaminated environment, be unfavorable for that people's is healthy, therefore, consider, adopt citric acid to control dye liquor pH value and dye again between 3.5 ~ 4.0, the Color of Polyester Fabric of Ultra-fine Fibre under Alkali Condition is best, and dyeing environmental protection.
Adopt levelling agent PRDN of the present invention, leveling agent d PS (enjoying this chemical industry advanced in years) under spectrophotometric determination condition of different temperatures and the absorbance of dye liquor before and after Polyester Fabric of Ultra-fine Fibre under Alkali Condition dyeing when not adding levelling agent, and calculate dye-uptake by formula (1), test result is shown in Fig. 4, Fig. 5, Fig. 6 respectively:
Dye-uptake (%)=(1-nA 1/ mA 0) × 100% (1)
In formula: the dye liquor extension rate that m/n-------dyes front/rear;
A 0/ A 1-----dye front/rear dye liquor dilution m/n doubly after absorbance.
As can be seen from Figure 6, between 100 DEG C ~ 130 DEG C, dye-uptake sharply rises, this very easily causes the irregular of dyeing, therefore, improve the level-dyeing property of fabric, just must slow down the dye-uptake of dyestuff, as can be seen from Fig. 4, Fig. 5, add levelling agent in dye liquor and can slow down the speed that dyestuff contaminates, be conducive to the dyeability improving super fine polyester.More mild than in Fig. 5 of adsorption curve in Fig. 4, therefore select levelling agent PRDN more suitable.And disperse gorgeous blue SWF (before dye liquor intensification) when sawing sheet to add the levelling agent PRDN of 2/3 consumption, and use boiling water sawing sheet, can effectively reduce gathering of dyestuff.And levelling agent PRDN in comparative example 5 is disposable before dye liquor heats up adds, in follow-up temperature-rise period, dyestuff easily flocks together.
As shown in Figure 4, disperse gorgeous blue SWF below 130 DEG C, along with the rising of temperature, test dye power part increases gradually, when being raised to 130 DEG C, dye-uptake reaches balance, holding time, sample dye-uptake no longer increases, and is incubated the level-dyeing property of 30 points of kinds to Polyester Fabric of Ultra-fine Fibre under Alkali Condition highly beneficial under 130 DEG C of conditions.Be raised to the temperature range of 90% by 15% relative to test dye, disperse gorgeous blue SWF to be roughly 100-130 DEG C, this warm area should be slow heating zone, and 100-110 DEG C controls heating rate is 1.0; 110 DEG C ~ 130 DEG C control heating rate is 0.5 DEG C/min.
Test the swelling agent DFM of variable concentrations in the steps below to the impact moving dye rate of the gorgeous blue SWF of dispersion, test result is in table 3:
(1) add lemon acid and direct dyes, do not add other auxiliary agent, matched well dye liquor by water.
(2) standby 3 pieces of 4 grams of Polyester Fabric of Ultra-fine Fibre under Alkali Conditions (cloth A, cloth B and cloth C), cloth A and cloth B together puts into dyeing temperature (130 DEG C) dip-dye 30 minutes.
(3) careful taking-up cloth A after cooling, extrudes dye liquor, dry cloth after reduction cleaning.
(4) 4 grams of grey cloth cloth C that the cloth B dyed is identical with another block, separately add clear water co-bathing dyeing and are incubated 30 minutes.
(5) careful taking-up cloth B and cloth C, extrudes dye liquor, dry cloth after reduction cleaning.
Surveying color matching system in cloth B with Datacolor is standard, and cloth C reads dynamics value to cloth B, and gained percentage is both for moving dye rate.
The swelling agent DFM of table 3. variable concentrations moves dye effect to the gorgeous blue SWF's of dispersion
Swelling agent concentration (g/L) 0 0.5 1.0 1.5 2.0 2.5 3
Move dye rate (%) 16 21 24 28 33 34 35
As can be seen from Table 3, when not adding swelling agent, the dye rate of moving of disperseing gorgeous blue SWF only 16%, and add swelling agent DFM can effectively improve dispersion gorgeous blue SWF move dye rate: when swelling agent DFM consumption is greater than 2g/L, move the increase of dye rate no longer obvious, consider cost, actual production selects the swelling agent DFM of 2g/L the most suitable.
Adopt Datacolor Computer color testing instrument to measure dye sample aberration △ E at D65 light source, △ E numerical value is all using Customer Standard colour table as reference colour.Testing example 1 ~ 5 and the dye sample aberration obtained by comparative example 3,5, test result is in table 4.
Table 4. Polyester Fabric of Ultra-fine Fibre under Alkali Condition low bath ratio dyeing colour stability
As shown in Table 4, adopt method of the present invention to dye, the color of Polyester Fabric of Ultra-fine Fibre under Alkali Condition can reach Customer Standard, and dyeing also can be up to standard with the color of cylinder, and Color is more satisfactory.And adding citric acid or levelling agent do not dye disposable adding again, the color aberration of obtained Polyester Fabric of Ultra-fine Fibre under Alkali Condition is very large.
Adopt the method dye Polyester Fabric of Ultra-fine Fibre under Alkali Condition 500Kg of embodiment 1, divide 20 by the Polyester Fabric of Ultra-fine Fibre under Alkali Condition contaminated, survey these 20 fabrics of color matching system with Datacolor and survey 555 color separations, the results are shown in Table 5.
The color difference analysis that table 5. Polyester Fabric of Ultra-fine Fibre under Alkali Condition low bath ratio dyeing manufactures a finished product greatly
Note: in table, 1-20 is cloth numbering.555Sort Code the 1st 5 represents the depth; Represent shading value for 2nd 5; Represent coloured light for 3rd 5.555 is the mean value of 1-20 the depth, shading value, coloured light.The gorgeous blue SWF of this cylinder DISPERSE DYES low bath raio dye Polyester Fabric of Ultra-fine Fibre under Alkali Condition 555Sort Code is 212 (differences of the maxima and minima that the depth, shading value, coloured light are every), and difference summation is 5 (2+1+2).Summation is less than 5 excellent, and 5 ~ 7 is up to standard, is greater than 7 and do not pass through.
From the data of table 5, the aberration manufactured a finished product greatly is all less than 7, and Color is desirable.
The wash water fastness of the dye sample obtained by AATCC Test Method 61-2008 testing example 1 ~ 3; The water of the dye sample obtained by AATCC Test Method 107-2008 testing example 1 ~ 3; The bleed fastness of the dye sample obtained by JIS Test Method " large ball method look tears fastness " testing example 1 ~ 3; The crock fastness of the dye sample obtained by AATCC Test Method 8-2003 testing example 1 ~ 3; Test result is in table 6.
Table 6. COLOR FASTNESS test result
As shown in Table 6, disperse gorgeous blue SWF to contaminate Polyester Fabric of Ultra-fine Fibre under Alkali Condition fabric fastness after post processing can control more than 4 grades.
In sum, method of the present invention is adopted to dye to Polyester Fabric of Ultra-fine Fibre under Alkali Condition, dye-uptake can be improved while the every COLOR FASTNESS of guarantee reaches more than 4 grades, prevent look flower, improve dyeability, prevent from disperseing, in gorgeous blue SWF dyeing high temperature temperature-fall period, Second Aggregation occurs, obtain desirable Color.
Above embodiment is only used for method detailed of the present invention is described, the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.

Claims (10)

1. the colouring method of a Polyester Fabric of Ultra-fine Fibre under Alkali Condition, it is characterized in that, comprise staining procedure: in the Polyester Fabric of Ultra-fine Fibre under Alkali Condition soaked, add softener, part levelling agent and swelling agent be made into working solution, and add pH adjusting agent adjustment working solution pH to 3.5 ~ 4.0, add DISPERSE DYES when being warming up to 43 DEG C and remain levelling agent and be made into dye liquor, then heat up dyeing.
2. colouring method according to claim 1, is characterized in that, described Polyester Fabric of Ultra-fine Fibre under Alkali Condition dyes in airflow dyeing machine, and dye bath ratio is 1:4 ~ 8.
3. colouring method according to claim 1, is characterized in that, the heating rate that described working solution is warming up to 43 DEG C is 3 DEG C/min; Described intensification dyeing adopts sectional type to heat up: control dye liquor with the ramp to 100 DEG C of 2 DEG C/min, then with the ramp to 110 DEG C of 0.8 DEG C/min, finally with DEG C insulation of the ramp to 130 of 1.8 DEG C/min.
4. colouring method according to claim 3, is characterized in that, linearly add DISPERSE DYES and residue levelling agent when described working solution is warming up to 43 DEG C again, the linear joining day of described DISPERSE DYES and residue levelling agent is 20min;
Described levelling agent is PRDN, and described part levelling agent is 0.5 ~ 4g/L with the consumption sum of residue levelling agent, and described part levelling agent is 2:1 with the mass ratio of residue levelling agent.
5. colouring method according to claim 1, is characterized in that, the consumption of described DISPERSE DYES is 0.6 ~ 6% (OWF);
Described softener is CN, and the consumption of described softener is 1 ~ 3g/L;
Described swelling agent is DFM, and the consumption of described swelling agent is 0.5 ~ 2g/L;
Described pH adjusting agent is citric acid, and the consumption of described pH adjusting agent is 0.5 ~ 1.2g/L.
6. colouring method according to claim 3, is characterized in that, the time of described 130 DEG C of insulations is 30min.
7. colouring method according to claim 3, it is characterized in that, also need to lower the temperature after described intensification dyeing, described cooling is sectional type cooling: after control dye liquor is cooled to 110 DEG C with 4 DEG C/min, be cooled to 95 DEG C with 2.5 DEG C/min, be finally cooled to 70 DEG C of drainings with 1.5 DEG C/min.
8. the colouring method according to any one of claim 1 to 7, is characterized in that, also comprises High Temperature Pre fixating shape step before described staining procedure: Polyester Fabric of Ultra-fine Fibre under Alkali Condition is placed in pre-setting machine, at 190 DEG C of pre-setting process 20 ~ 30s.
9. the colouring method according to any one of claim 1 to 7, it is characterized in that, also reduction clearing step is comprised: add water and NaOH is made into cleaning fluid after described staining procedure, cleaning fluid takes a policy after being warming up to 60 DEG C powder process, then the cleaning fluid controlled after sodium hydrosulfite process is warming up to 85 DEG C of insulations, be cooled to 70 DEG C of drainings again, also need after draining to carry out neutralisation treatment to Polyester Fabric of Ultra-fine Fibre under Alkali Condition.
10. colouring method according to claim 9, is characterized in that, the consumption of described NaOH is 4 ~ 6g/L;
The heating rate that described cleaning fluid is warming up to 60 DEG C is 4 DEG C/min;
The heating rate that cleaning fluid after sodium hydrosulfite process is warming up to 85 DEG C is 3 DEG C/min, and temperature retention time is 9min;
Described sodium hydrosulfite adds at twice: first add 1/2 sodium hydrosulfite insulation 3min, and then add residue 1/2 sodium hydrosulfite insulation 3min;
The rate of temperature fall that described cleaning fluid is cooled to 70 DEG C is 1.5 DEG C/min;
Described neutralisation treatment comprises: in the Polyester Fabric of Ultra-fine Fibre under Alkali Condition after draining, add water and 0.3g/L citric acid, with draining after the ramp to 70 of 3 DEG C/min DEG C cleaning 5min, then adds water and 0.2g/L citric acid, draining after cleaning 5min.
CN201510266835.6A 2015-05-21 2015-05-21 Method for dyeing superfine terylene fabric Active CN104878618B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510266835.6A CN104878618B (en) 2015-05-21 2015-05-21 Method for dyeing superfine terylene fabric

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510266835.6A CN104878618B (en) 2015-05-21 2015-05-21 Method for dyeing superfine terylene fabric

Publications (2)

Publication Number Publication Date
CN104878618A true CN104878618A (en) 2015-09-02
CN104878618B CN104878618B (en) 2017-03-22

Family

ID=53946282

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510266835.6A Active CN104878618B (en) 2015-05-21 2015-05-21 Method for dyeing superfine terylene fabric

Country Status (1)

Country Link
CN (1) CN104878618B (en)

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105200812A (en) * 2015-10-20 2015-12-30 互太(番禺)纺织印染有限公司 Dyeing process of using dispersal fluorescent dye to dye super-fine polyester elastic fabric
CN105970670A (en) * 2016-06-23 2016-09-28 西安工程大学 Preparation method and application of leveling agent for high-temperature and high-pressure dyeing of polyester fibers by disperse dyes
WO2017075942A1 (en) * 2015-11-03 2017-05-11 江苏新凯盛企业发展有限公司 Dyeing and finishing method for manufacturing fabric by using heat absorbable heating material
CN106702767A (en) * 2016-11-28 2017-05-24 恩平锦兴纺织印染企业有限公司 Preparation method of knitted fabric with one-way moisture conduction and cooling functions
CN106978733A (en) * 2017-04-01 2017-07-25 际华三五四三针织服饰有限公司 Polyester elastic cloth royalblue airflow dyeing technique
CN107254751A (en) * 2017-05-27 2017-10-17 浙江银河印染有限公司 A kind of method for eliminating the low bath raio airflow dyeing wrinkle of polyamide fibre people's cotton spandex Roman cloth
CN107489046A (en) * 2017-09-06 2017-12-19 互太(番禺)纺织印染有限公司 A kind of dyeing and finishing technology of dacron
CN108779602A (en) * 2016-01-04 2018-11-09 尼克瓦格斯有限公司 improved method for removing textile dyes
CN109162127A (en) * 2018-06-23 2019-01-08 浙江绿洲印染有限公司 A kind of printing technology and the spray thrower applied to printing technology process
CN109355942A (en) * 2018-09-14 2019-02-19 桐乡市濮院毛针织技术服务中心 A kind of rose dyeing of dacron preparation method of dispersing agent
CN109594356A (en) * 2018-11-26 2019-04-09 福建信泰印染有限公司 It is a kind of to wash the/dyeing of the two-sided Jacquard footwear material fabric of brocade
CN109695117A (en) * 2017-10-24 2019-04-30 石狮市新祥华染整发展有限公司 A method of overcome superfine fibre cloth because of folding line caused by dyeing
CN109778570A (en) * 2019-01-04 2019-05-21 温州中普纺织有限公司 A kind of super fine polyester silk colouring method
CN110284346A (en) * 2019-07-04 2019-09-27 闽江学院 A kind of terylene and its colouring method of carbon nanotubes
CN111058168A (en) * 2019-12-31 2020-04-24 江苏金辰针纺织有限公司 Preparation method of knitted fabric with moisture absorption, sweat releasing and continuous cool feeling functions
CN111235906A (en) * 2020-01-16 2020-06-05 浙江稽山印染有限公司 Dyeing process of suede nap
CN111235920A (en) * 2020-01-21 2020-06-05 互太(番禺)纺织印染有限公司 Dyeing process of regenerated polyester
CN111350084A (en) * 2020-03-11 2020-06-30 嘉兴市天伦纳米染整有限公司 Terylene four-side elastic high-fastness dyeing processing technology
CN112301760A (en) * 2020-11-04 2021-02-02 郎溪远华纺织有限公司 Dyeing process of moisture-absorbing quick-drying polyester fabric
CN113026173A (en) * 2021-04-14 2021-06-25 桐乡市天利织造有限公司 Production process of soft-hand-feeling suede nap fabric
CN113295639A (en) * 2021-06-15 2021-08-24 杭州美高华颐化工有限公司 Method for testing high-temperature dispersibility of leveling agent for disperse dye
CN113832582A (en) * 2021-08-26 2021-12-24 江阴市茂达棉纺厂有限公司 Composite yarn and preparation and coloring method thereof
CN113846414A (en) * 2021-11-03 2021-12-28 绍兴华欣布艺有限公司 Production method of polylactic acid fiber and polyester blended warp-knitted fabric
CN114763678A (en) * 2022-04-18 2022-07-19 圣山集团有限公司 Dyeing method of polyester fabric for high-color-fastness luggage fabric
CN114855470A (en) * 2022-04-15 2022-08-05 圣山集团有限公司 Gray dye for light-dyed polyester fabric and dyeing process thereof
CN115161866A (en) * 2022-05-20 2022-10-11 嘉兴华绰纺织股份有限公司 Production process of warp knitting hydrophobic polyester fabric

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101144248A (en) * 2007-10-18 2008-03-19 江苏盛虹化纤有限公司 Method for dyeing ultra-fine denier dacron vividly and equally
CN102628211A (en) * 2012-04-16 2012-08-08 盛虹集团有限公司 Novel dyeing and finishing processing technology of micro polyester fabric
CN103225213A (en) * 2013-05-16 2013-07-31 吴江创新印染厂 Dyeing technology
CN104233851A (en) * 2014-09-09 2014-12-24 上海嘉麟杰纺织品股份有限公司 Method for staining superfine polyester fabric by use of FORON CYANIE S-WF as main dye

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101144248A (en) * 2007-10-18 2008-03-19 江苏盛虹化纤有限公司 Method for dyeing ultra-fine denier dacron vividly and equally
CN102628211A (en) * 2012-04-16 2012-08-08 盛虹集团有限公司 Novel dyeing and finishing processing technology of micro polyester fabric
CN103225213A (en) * 2013-05-16 2013-07-31 吴江创新印染厂 Dyeing technology
CN104233851A (en) * 2014-09-09 2014-12-24 上海嘉麟杰纺织品股份有限公司 Method for staining superfine polyester fabric by use of FORON CYANIE S-WF as main dye

Cited By (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105200812A (en) * 2015-10-20 2015-12-30 互太(番禺)纺织印染有限公司 Dyeing process of using dispersal fluorescent dye to dye super-fine polyester elastic fabric
WO2017075942A1 (en) * 2015-11-03 2017-05-11 江苏新凯盛企业发展有限公司 Dyeing and finishing method for manufacturing fabric by using heat absorbable heating material
CN108779602A (en) * 2016-01-04 2018-11-09 尼克瓦格斯有限公司 improved method for removing textile dyes
CN105970670A (en) * 2016-06-23 2016-09-28 西安工程大学 Preparation method and application of leveling agent for high-temperature and high-pressure dyeing of polyester fibers by disperse dyes
CN106702767A (en) * 2016-11-28 2017-05-24 恩平锦兴纺织印染企业有限公司 Preparation method of knitted fabric with one-way moisture conduction and cooling functions
CN106978733A (en) * 2017-04-01 2017-07-25 际华三五四三针织服饰有限公司 Polyester elastic cloth royalblue airflow dyeing technique
CN107254751A (en) * 2017-05-27 2017-10-17 浙江银河印染有限公司 A kind of method for eliminating the low bath raio airflow dyeing wrinkle of polyamide fibre people's cotton spandex Roman cloth
CN107489046A (en) * 2017-09-06 2017-12-19 互太(番禺)纺织印染有限公司 A kind of dyeing and finishing technology of dacron
CN109695117A (en) * 2017-10-24 2019-04-30 石狮市新祥华染整发展有限公司 A method of overcome superfine fibre cloth because of folding line caused by dyeing
CN109162127B (en) * 2018-06-23 2020-12-22 浙江绿洲印染有限公司 Printing process
CN109162127A (en) * 2018-06-23 2019-01-08 浙江绿洲印染有限公司 A kind of printing technology and the spray thrower applied to printing technology process
CN109355942A (en) * 2018-09-14 2019-02-19 桐乡市濮院毛针织技术服务中心 A kind of rose dyeing of dacron preparation method of dispersing agent
CN109594356A (en) * 2018-11-26 2019-04-09 福建信泰印染有限公司 It is a kind of to wash the/dyeing of the two-sided Jacquard footwear material fabric of brocade
CN109778570A (en) * 2019-01-04 2019-05-21 温州中普纺织有限公司 A kind of super fine polyester silk colouring method
CN110284346A (en) * 2019-07-04 2019-09-27 闽江学院 A kind of terylene and its colouring method of carbon nanotubes
CN111058168A (en) * 2019-12-31 2020-04-24 江苏金辰针纺织有限公司 Preparation method of knitted fabric with moisture absorption, sweat releasing and continuous cool feeling functions
CN111235906A (en) * 2020-01-16 2020-06-05 浙江稽山印染有限公司 Dyeing process of suede nap
CN111235920A (en) * 2020-01-21 2020-06-05 互太(番禺)纺织印染有限公司 Dyeing process of regenerated polyester
CN111350084A (en) * 2020-03-11 2020-06-30 嘉兴市天伦纳米染整有限公司 Terylene four-side elastic high-fastness dyeing processing technology
CN112301760A (en) * 2020-11-04 2021-02-02 郎溪远华纺织有限公司 Dyeing process of moisture-absorbing quick-drying polyester fabric
CN113026173A (en) * 2021-04-14 2021-06-25 桐乡市天利织造有限公司 Production process of soft-hand-feeling suede nap fabric
CN113295639A (en) * 2021-06-15 2021-08-24 杭州美高华颐化工有限公司 Method for testing high-temperature dispersibility of leveling agent for disperse dye
CN113832582A (en) * 2021-08-26 2021-12-24 江阴市茂达棉纺厂有限公司 Composite yarn and preparation and coloring method thereof
CN113846414A (en) * 2021-11-03 2021-12-28 绍兴华欣布艺有限公司 Production method of polylactic acid fiber and polyester blended warp-knitted fabric
CN114855470A (en) * 2022-04-15 2022-08-05 圣山集团有限公司 Gray dye for light-dyed polyester fabric and dyeing process thereof
CN114763678A (en) * 2022-04-18 2022-07-19 圣山集团有限公司 Dyeing method of polyester fabric for high-color-fastness luggage fabric
CN115161866A (en) * 2022-05-20 2022-10-11 嘉兴华绰纺织股份有限公司 Production process of warp knitting hydrophobic polyester fabric

Also Published As

Publication number Publication date
CN104878618B (en) 2017-03-22

Similar Documents

Publication Publication Date Title
CN104878618B (en) Method for dyeing superfine terylene fabric
CN103132349B (en) Dyeing and finishing method of superfine denier nylon fabric
CN105200812B (en) Dyeing process of using dispersal fluorescent dye to dye super-fine polyester elastic fabric
CN103132350B (en) Manufacturing method of polyester-silk interwoven fabrics
CN103525123B (en) Nylon sea-island microfiber leather fabric composite dye and application thereof
CN104532460B (en) The processing method of the interval knitting bubble fabric of transfer printing
CN104532611A (en) Method for printing and dyeing dacron/chinlon/cotton/spandex multi-component fiber fabric
CN109371721A (en) Complete cotton knitted fabric dyeing production technology
CN109680514A (en) A kind of dyeing for washing ammonia four sides elasticity fabric
CN104631156B (en) Real silk/T400 fabric one-bath one-step dyeing dyeing and finishing technology
CN104762839A (en) Low-temperature dyeing process of nylon/Dacron elastic knitted fabric
CN109554911A (en) A kind of dyeing and finishing processing method of 400 fabric of memory T based on bio-based materials
CN107385958A (en) A kind of dyeing and finishing technology of fiber blend color-woven fabric
CN101413207B (en) Dyeing and finishing process for sea silk fabric
CN105256603B (en) The dyeing and finishing method of fabric is made in a kind of exothermic material that absorbs heat
CN103981746A (en) Homochromatic dyeing process of wool/acrylic fiber blended fabric
CN110344262A (en) A kind of dyeing of dacron is with water-proof finish with one step processing method of bath
CN103469632B (en) A kind of colouring method of super imitative cotton cashmere blended fabrics
CN109505149A (en) It is a kind of based on bio-based materials through the dyeing and finishing processing method to cationic T400 fabric
CN102995470A (en) Preparation method for durable ultraviolet-proof dacron fabric
CN104018363A (en) Dyeing process of superfine denier acrylon knitted fabric
CN106120331A (en) A kind of terylene and the moisture absorbable and breathable finishing method of chinlon blended fabric
CN105803825A (en) Dyeing process for cotton and linen fabric
CN108385409A (en) A kind of raw silk/Eco-wash wools(Mercerising)Wool interwoven fabric Tone-on-Tone Dyeing method
CN101492850A (en) Dyeable dacron textile containing cationic dye and production method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
EXSB Decision made by sipo to initiate substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant