CN109518493A - A kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing of energy-saving and emission-reduction - Google Patents
A kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing of energy-saving and emission-reduction Download PDFInfo
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- CN109518493A CN109518493A CN201811380301.6A CN201811380301A CN109518493A CN 109518493 A CN109518493 A CN 109518493A CN 201811380301 A CN201811380301 A CN 201811380301A CN 109518493 A CN109518493 A CN 109518493A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3271—Hydroxyamines
- C08G18/3275—Hydroxyamines containing two hydroxy groups
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6648—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6655—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6688—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/82—Textiles which contain different kinds of fibres
- D06P3/8204—Textiles which contain different kinds of fibres fibres of different chemical nature
- D06P3/8223—Textiles which contain different kinds of fibres fibres of different chemical nature mixtures of fibres containing hydroxyl and ester groups
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing of energy-saving and emission-reduction, by polyester polyol or polyether polyols and hard segment regulator TX and IPDI, HDI and/or TDI, reaction obtains performed polymer, performed polymer is reacted with acetone and chain extender R, again through self-emulsifying, color fixing agent product is finally obtained.Color fixing agent obtained can significantly improve the color fastness to washing and resistance to dry, fastness to wet rubbing of polyester cotton through the invention, and finishing effect has good water resistance, environmentally protective.Key is that the color fixing agent can be added directly during cotton-polyester blended fabric co-bathing dyeing, without dye after carry out fixation, simplify process flow, have highly important meaning for energy-saving and emission-reduction.
Description
The application is application number: 201710228449.7, the applying date: 2017-04-10, a kind of title " cotton-polyester blended fabric
The divisional application of the dedicated color fixing agent of co-bathing dyeing ".
Technical field
The present invention relates to a kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing.
Background technique
Cotton-polyester blended fabric co-bathing dyeing multiselect reactive dye and disperse dyes, since reactive dye are intolerant to bleaching, no
It easily strips, maximum weakness is dyestuff using not exclusively, and most active dyestuff all can be anti-along with hydrolysis in dyeing course
The generation answered, hydrolised dye will form loose colour in fabric surface, cause in Fabrics Dyed with Reactive Dyes, especially blended yarn weaved fabric,
The color fastness to washing of deep-colour fabric and it is resistance to it is dry, fastness to wet rubbing is poor, generally only 1~2 grade, it is difficult to reach international or country
Relevant criterion.And some finishing agents currently on the market are usually monistic finishing auxiliaries, raising that can only be single is washable
Color fastness or resistance to dry, fastness to wet rubbing, and be that final finishing is carried out after textile dyeing, do not meet what country at present was proposed
The requirement of energy-saving and emission-reduction.
The color fastness to washing of dyed fabric and resistance to dry, wet can be improved with multi-functional compound processing cotton-polyester blended fabric
Crock fastness.The present invention has synthesized a kind of color fixing agent NMMP, and be used for improve cotton-polyester blended fabric color fastness to washing and
Resistance to dry, fastness to wet rubbing.It is proved by a large amount of application experiment and performance test, they are improving the washable of cotton-polyester blended fabric
It works well in terms of color fastness and resistance to dry, fastness to wet rubbing.Meanwhile other yarn dyed fabrics are equally applicable to, such as directly, vulcanizes, is weak
The improvement of the color fastness to washing of acid dyeing fabric and resistance to dry, fastness to wet rubbing etc..The color fixing agent that the present invention synthesizes
NMMP forms reticulated film in fiber surface, covers and closes off dyestuff, prevent fabric from taking when it acts on fabric
Dyestuff occurs in journey to be swollen, dissolve, fall off, stain, improves color fastness to washing and resistance to dry, fastness to wet rubbing mesh to reach
's.
Summary of the invention
The purpose of the present invention is to provide a kind of color fastness to washings for improving polyester-cotton blend co-bathing dyeing blended yarn weaved fabric and resistance to dry, wet
The dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing of crock fastness.
The technical solution of the invention is as follows:
A kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing, it is characterized in that: being made of following method:
Step 1: polyester polyol or polyether polyols and hard segment regulator TX being placed in three-necked flask, 100-
Dehydration 1-10h is vacuumized at 200 DEG C；
Step 2: being filled with nitrogen protection into the three-necked flask of step 1, and thermometer and blender are installed on three-necked flask；
Step 3: at 30-90 DEG C, toward through vacuum dehydration and nitrogen protection polyester polyol or polyether polyols in
Be added IPDI, HDI and/or TDI, react 1-10h after, obtain-NCO content close to theoretical value NCO end group performed polymer；
Step 4: it takes the performed polymer of 1-1.5g to react in toluene solution with excessive di-n-butylamine, generates corresponding substituted urea,
After the reaction was completed, remaining di-n-butylamine is titrated with HCl standard solution, measures-NCO content；
Step 5: 10-100g acetone soln being added in the performed polymer prepared in step 3, chain extender R and third is added dropwise at 30-80 DEG C
The mixed solution of ketone；Chain extender R and acetone quality ratio are 1:1-10 in the mixed solution of the chain extender R and acetone, and 1-5 is small
When interior be added dropwise to complete；
Step 6: the reaction was continued at 30-80 DEG C after completion of dropwise addition 1-5h prepares polyesters compound；
Step 7: 20-200g deionized water being added in polyesters compound obtained into step 6 and carries out self-emulsifying, finally obtains
Color fixing agent product；
The hard segment regulator TX is the mixture of ethylene glycol, glycerine and 1,4-butanediol, and ethylene glycol, glycerine and 1,
The mass ratio of 4- butanediol is 1-10:1-10:1-10；The chain extender R is the mixing of N-methyl diethanolamine and hydroxy silicon oil
Object, and N-methyl diethanolamine and hydroxy silicon oil mass ratio are 1-10:1-10.
The polyester polyol or polyether polyols be PEG-400, PEG600, PEG1000, PEG1500,
One or more of GE210, GE310.
In described IPDI, HDI, TDI-and NCO and-OH molar ratio :-NCO :-OH=2-8:1.
The quality that the mixed solution of chain extender R and acetone is added dropwise in step 5 is 5-20 grams.
In step 1 mass ratio of polyester polyol or polyether polyols and hard segment regulator TX be 1 ~ 10:1 ~
10, total dosage of polyester polyol or polyether polyols and hard segment regulator TX are 10 ~ 50 parts by weight；In step 3
The dosage of IPDI, HDI and/or TDI are 5 ~ 20 parts by weight.
The beneficial effects of the present invention are: color fixing agent NMMP obtained can significantly improve polyester cotton through the invention
Color fastness to washing and resistance to dry, fastness to wet rubbing, and finishing effect has good water resistance, it is environmentally protective.Key is the fixation
Agent can be added directly during cotton-polyester blended fabric co-bathing dyeing and (is added in dye liquor, additional amount is 10 ~ 50g/L), without
Fixation is carried out after dyeing, simplifies process flow, has highly important meaning for energy-saving and emission-reduction.
Below with reference to embodiment, the invention will be further described.
Specific embodiment
Embodiment 1:
PEG1500 and hard segment regulator TX are placed in three-necked flask by step 1, and dehydration 3h is vacuumized at 120 DEG C.
Total dosage of PEG1500 and hard segment regulator TX are that the mass ratio of 20g, PEG1500 and hard segment regulator TX are 1:1；
Step 2 is filled with nitrogen protection into the three-necked flask of step 1, and thermometer and blender are installed on three-necked flask.
Step 3, at 80 DEG C, be added into PEG1500 and hard segment regulator TX through vacuum dehydration and nitrogen protection
TDI (molar ratio-NCO :-OH=2:1), react 2h after, obtain-NCO content close to theoretical value NCO end group pre-polymerization
Body.The dosage of TDI is 6g；
Step 4 takes the performed polymer of 1-1.5g to react in toluene solution with excessive di-n-butylamine, generates corresponding substituted urea,
After the reaction was completed, remaining di-n-butylamine is titrated with HCl standard solution, measures-NCO content.
10g acetone soln is added in step 5, the performed polymer prepared in step 3, be added dropwise at 50 DEG C 10 grams of chain extender R with
(chain extender R is 1:4) with acetone quality ratio to the mixed solution of acetone, is added dropwise to complete in 1h.
The reaction was continued at 50 DEG C after step 6, completion of dropwise addition 1h, prepares the polyesters chemical combination with certain molecular weight
Object.
About 100g deionized water progress self-emulsifying is added into step 6 for step 7 in obtained polyesters compound, adjust body
The active constituent content of system is 20%, finally obtains color fixing agent.Color fixing agent addition is same in the polyester cotton of dark color system
It bathes in dyeing course and (is added in dye liquor, additional amount 20g/L), test result is its color fastness to washing (staining grade and colour fading
Grade) 1 grade is improved, fastness to wet rubbing improves 1.5 grades.
Embodiment 2
GE210 and hard segment regulator TX are placed in three-necked flask by step 1, and dehydration 1.5h is vacuumized at 130 DEG C.GE210
And it is 1:5 that the sum of dosage of hard segment regulator TX, which is the mass ratio of 40g, GE210 and hard segment regulator TX,.
Step 2 is filled with nitrogen protection into the three-necked flask of step 1, and thermometer and stirring are installed on three-necked flask
Device.
Step 3, at 70 DEG C, be added into GE210 and hard segment regulator TX through vacuum dehydration and nitrogen protection
15gHDI (- NCO :-OH=2:1), react 3h after, obtain-NCO content close to theoretical value NCO end group performed polymer.
Step 4 takes the performed polymer of 1-1.5g to react in toluene solution with excessive di-n-butylamine, generates corresponding replace
Urea titrates remaining di-n-butylamine with HCl standard solution, measures-NCO content after the reaction was completed.
10g acetone soln is added in step 5, the performed polymer prepared in step 3, be added dropwise at 30 DEG C 20 grams of chain extender R with
(chain extender R is 1:4) with acetone quality ratio to the mixed solution of acetone, is added dropwise to complete in 2h.
The reaction was continued at 30 DEG C after step 6, completion of dropwise addition 3h, prepares the polyesters chemical combination with certain molecular weight
Object.
About 100g deionized water progress self-emulsifying is added into step 6 for step 7 in obtained polyesters compound, adjust body
The active constituent content of system is 20%, finally obtains color fixing agent NMMP.Polyester-cotton blend by color fixing agent addition in dark color system blended is knitted
During object co-bathing dyeing (be added dye liquor in, additional amount 50g/L), test result be its color fastness to washing (staining grade and
Colour fading grade) 1 grade is improved, fastness to wet rubbing improves 1.5 grades.
Embodiment 3
GE310 and hard segment regulator TX are placed in three-necked flask by step 1, and dehydration 2h is vacuumized at 120 DEG C.GE310 and hard
The sum of dosage of segment regulator TX is that the mass ratio of 50g, GE310 and hard segment regulator TX are 5:1.
Step 2 is filled with nitrogen protection into the three-necked flask of step 1, and thermometer and stirring are installed on three-necked flask
Device.
Step 3, at 50 DEG C, 10g is added into GE310 and hard segment regulator TX through vacuum dehydration and nitrogen protection
IPDI (- NCO :-OH=2:1), react 3h after, obtain-NCO content close to theoretical value NCO end group performed polymer.
Step 4 takes the performed polymer of 1-1.5g to react in toluene solution with excessive di-n-butylamine, generates corresponding replace
Urea titrates remaining di-n-butylamine with HCl standard solution, measures-NCO content after the reaction was completed.
10g acetone soln is added in step 5, the performed polymer prepared in step 3, be added dropwise at 40 DEG C 15 grams of chain extender R with
(chain extender R is 1:3) with acetone quality ratio to the mixed solution of acetone, is added dropwise to complete in 1h.
The reaction was continued at 40 DEG C after step 6, completion of dropwise addition 2h, prepares the polyesters chemical combination with certain molecular weight
Object.
About 100g deionized water progress self-emulsifying is added into step 6 for step 7 in obtained polyesters compound, adjust body
The active constituent content of system is 20%, finally obtains color fixing agent NMMP.Polyester-cotton blend by color fixing agent addition in dark color system blended is knitted
During object co-bathing dyeing (be added dye liquor in, additional amount 30g/L), test result be its color fastness to washing (staining grade and
Colour fading grade) 1 grade is improved, fastness to wet rubbing improves 1.5 grades.
Claims (1)
1. a kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing of energy-saving and emission-reduction, it is characterized in that: being made of following method:
GE210 and hard segment regulator TX are placed in three-necked flask by step 1, and dehydration 1.5h is vacuumized at 130 DEG C；GE210
And it is 1:5 that the sum of dosage of hard segment regulator TX, which is the mass ratio of 40g, GE210 and hard segment regulator TX,；
Step 2 is filled with nitrogen protection into the three-necked flask of step 1, and thermometer and blender are installed on three-necked flask；
Step 3, at 70 DEG C, 15gHDI is added into GE210 and hard segment regulator TX through vacuum dehydration and nitrogen protection
(- NCO :-OH=2:1), react 3h after, obtain-NCO content close to theoretical value NCO end group performed polymer；
Step 4 takes the performed polymer of 1-1.5g to react in toluene solution with excessive di-n-butylamine, generates corresponding substituted urea,
After the reaction was completed, remaining di-n-butylamine is titrated with HCl standard solution, measures-NCO content；
10g acetone soln is added in step 5, the performed polymer prepared in step 3,20 grams of chain extender R and acetone is added dropwise at 30 DEG C
Mixed solution (chain extender R and acetone quality ratio be 1:4), be added dropwise to complete in 2h；
The reaction was continued at 30 DEG C after step 6, completion of dropwise addition 3h, prepares the polyesters compound with certain molecular weight；
About 100g deionized water progress self-emulsifying is added into step 6 for step 7 in obtained polyesters compound, regulation system
Active constituent content is 20%, finally obtains color fixing agent NMMP.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811380301.6A CN109518493B (en) | 2017-04-10 | 2017-04-10 | Energy-saving emission-reducing color fixing agent special for one-bath dyeing of polyester-cotton blended fabric |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811380301.6A CN109518493B (en) | 2017-04-10 | 2017-04-10 | Energy-saving emission-reducing color fixing agent special for one-bath dyeing of polyester-cotton blended fabric |
| CN201710228449.7A CN106917308B (en) | 2017-04-10 | 2017-04-10 | A kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing |
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| CN201710228449.7A Division CN106917308B (en) | 2017-04-10 | 2017-04-10 | A kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing |
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| CN201710228449.7A Active CN106917308B (en) | 2017-04-10 | 2017-04-10 | A kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing |
| CN201811380398.0A Active CN109518494B (en) | 2017-04-10 | 2017-04-10 | Preparation method of color fixing agent special for one-bath dyeing of polyester-cotton blended fabric |
| CN201811380301.6A Active CN109518493B (en) | 2017-04-10 | 2017-04-10 | Energy-saving emission-reducing color fixing agent special for one-bath dyeing of polyester-cotton blended fabric |
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| CN201710228449.7A Active CN106917308B (en) | 2017-04-10 | 2017-04-10 | A kind of dedicated color fixing agent of cotton-polyester blended fabric co-bathing dyeing |
| CN201811380398.0A Active CN109518494B (en) | 2017-04-10 | 2017-04-10 | Preparation method of color fixing agent special for one-bath dyeing of polyester-cotton blended fabric |
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| CN110387029A (en) * | 2019-08-01 | 2019-10-29 | 南通市联缘染业有限公司 | A kind of preparation method of the dedicated color fixing agent of anionic cotton cheese dyeing |
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| CN109183468A (en) * | 2018-09-14 | 2019-01-11 | 桐乡市濮院毛针织技术服务中心 | A kind of polyester-cotton fabric black-dyeing color fixing agent |
| CN109355946A (en) * | 2018-09-14 | 2019-02-19 | 桐乡市濮院毛针织技术服务中心 | A kind of preparation method of polyester-cotton fabric black-dyeing color fixing agent |
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| CN109518494A (en) | 2019-03-26 |
| CN109518494B (en) | 2021-02-26 |
| CN106917308A (en) | 2017-07-04 |
| CN109518493B (en) | 2021-02-23 |
| CN109537332A (en) | 2019-03-29 |
| CN106917308B (en) | 2019-01-15 |
| CN109537332B (en) | 2021-07-20 |
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