CN111320757B - Preparation method of high-fastness ultralow-yellowing silicone oil for polyester fabric and polyester fabric - Google Patents
Preparation method of high-fastness ultralow-yellowing silicone oil for polyester fabric and polyester fabric Download PDFInfo
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- CN111320757B CN111320757B CN201811532187.4A CN201811532187A CN111320757B CN 111320757 B CN111320757 B CN 111320757B CN 201811532187 A CN201811532187 A CN 201811532187A CN 111320757 B CN111320757 B CN 111320757B
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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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/388—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
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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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
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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
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
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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
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5264—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds
- D06P1/5292—Macromolecular compounds obtained otherwise than by reactions involving only unsaturated carbon-to-carbon bonds containing Si-atoms
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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
- 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
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
- D06P3/54—Polyesters using dispersed dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Abstract
A preparation method of high-fastness ultralow-yellowing silicone oil for polyester fabrics comprises the following steps: 1) adding hydrogen-containing polysiloxane and allyl glycidyl ether at two ends into a flask, adding chloroplatinic acid catalyst, stirring, heating, stopping reaction until a characteristic absorption peak of a Si-H bond disappears, and removing excessive allyl glycidyl ether from a synthesized product to obtain linear epoxy-terminated polysiloxane; 2) adding epoxy-terminated polydimethylsiloxane and anhydrous piperazine with a quantitative molar ratio and a small molecular weight, and adding ethanol to obtain an ethanol solution of the epoxy-terminated polydimethylsiloxane at the two ends; 3) according to the molar ratio of the anhydrous piperazine to the dimethyl sulfate of 1: 2, adding an ethanol solution of double-end epoxy group polydimethylsiloxane with large molecular weight and dimethyl sulfate, stirring, heating, and keeping the temperature for 14 hours to obtain light yellow quaternized polydimethylsiloxane; 4) adding 100 g of quaternized modified epoxy-terminated silicone oil and a certain amount of emulsifier, adding warm water, and stirring to keep the system in a water-in-oil state; warm water was added dropwise.
Description
Technical Field
The invention relates to a preparation method of high-fastness ultralow-yellowing silicone oil for polyester fabrics and the polyester fabrics.
Background
Along with the development of times and social progress, the requirements of people on mental civilization construction and material civilization are higher and higher, and the requirements are particularly shown on the living level, the people can wear clothes, step by step and standard by year, for example, the problems of weaving defects and dyeing defects such as dyeing defects, dyeing spots, reed roads and the like which can be easily passed by more than ten years do not exist at present, customers can add new requirements of new standards every year, slight color cast flowers are reworked and repaired, serious re-production is carried out, the cost is increased, the profit is not realized, and the living space of a dye factory is reduced.
At the present stage, a lot of methods are used for softening and smoothing polyester fabrics, pretreatment alkali is reduced, a softening agent is added in after-treatment, the alkali reduction can cause the increase of a large amount of sewage COD, the gram weight of the fabrics can be reduced, the most used method is to add the softening agent, and in the softening agent, the direct-numbered organosilicone with the easiest handfeel, the highest adjustment performance and the highest cost ratio exists. The problems causing the fabric color change are mainly the following: 1. phenolic antioxidants such as BHT substances added to packaging materials are released during storage and transferred to fabrics, which undergo complex chemical reactions with nitrogen-containing oxides to form yellow substances that yellow the fabrics. 2. The amino group in the silicone oil chain segment reacts with the oxide in the air to cause yellowing, and the degree is more severe when the silicone oil is shaped at high temperature. 3. The emulsifier solvent in the silicone oil extracts the dye in the fabric, so that the dye is dissolved out of the surface, the fabric is yellowed, and the color fastness is reduced.
Many modified silicone oils or current terpolymer silicone oils on the market can give consideration to both yellowing and hand feeling of fabrics, but the color fastness has large loss, and in the placing process, the fabrics are in contact with oxides in the air, so that the potential risk of yellowing is caused, the factors are aggravated along with the increase of the using amount, and the requirements of customers with high-requirement strict standards can not be met.
Disclosure of Invention
The invention aims to provide a preparation method of high-fastness ultralow-yellowing silicone oil for polyester fabrics and the polyester fabrics, which have the advantages of high fastness and low yellowing, and overcome the defects of the prior art.
The technical scheme for solving the technical problem is as follows: a preparation method of high-fastness ultralow-yellowing silicone oil for polyester fabrics comprises the following steps:
1) adding hydrogen-containing polysiloxane and allyl glycidyl ether at two ends into a four-neck flask with a thermometer according to a certain molar ratio, uniformly stirring and heating to 85 ℃, adding 50ppm chloroplatinic acid catalyst (calculated according to the active ingredients of the chloroplatinic acid), uniformly stirring and mixing, heating to 100 ℃, keeping the temperature for 4 hours, and stopping the reaction until the characteristic absorption peak of the Si-H bond disappears. Removing excessive allyl glycidyl ether after the synthetic product is subjected to reduced pressure distillation to obtain colorless, clear and transparent linear double-end epoxy polysiloxane;
2) adding epoxy-terminated polydimethylsiloxane and anhydrous piperazine with a quantitative molar ratio and a small molecular weight into a four-neck flask with a thermometer, adding ethanol with the mass of 30% of that of the epoxy-terminated polydimethylsiloxane, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain a colorless, clear and transparent ethanol solution of double-end epoxy-group polydimethylsiloxane with a large molecular weight;
3) in a four-neck flask with a thermometer, adding a solvent according to a molar ratio of anhydrous piperazine to dimethyl sulfate of 1: 2, adding an ethanol solution of double-end epoxy group polydimethylsiloxane with large molecular weight and dimethyl sulfate, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain light yellow quaternized polydimethylsiloxane;
4) adding 100 g of quaternized modified epoxy-terminated silicone oil and a certain amount of emulsifier into a plastic beaker at one time, and putting the beaker into a constant-temperature water bath at 60 ℃ for heat preservation to 60 ℃; taking out the plastic beaker, adding about 10g of 60 ℃ warm water, and uniformly stirring the materials by using a glass rod; at this time, the viscosity of the material begins to increase slowly, and the system is still in a water-in-oil state; slowly adding about 18g of 60 ℃ warm water by using a dropper while stirring, and adding one dropper each time; at this time, the viscosity of the material is obviously increased to about 10g, and the viscosity of the material reaches the maximum and then gradually decreases.
In step 4), the material is subjected to a phase inversion process, in particular from water-in-oil to oil-in-water. In the process, water addition cannot be too fast, the next drop of pipe water can be added after the materials are fully stirred after each drop of pipe water is added, if the water addition is too fast, a system does not pass through the highest peak of viscosity, phase inversion is not sufficient, the particle size of the final emulsion is larger or the particle size distribution range is too wide, and the stability of the emulsion and even the application performance of the emulsion are affected; when a proper amount of water is added into the system while stirring, the system has good fluidity, the water adding speed in the process can be relatively high, because the material phase inversion is completed at the moment, the process is only a thinning process, and the particle size distribution of the emulsion are determined.
The polyester fabric is prepared by applying the high-fastness ultralow-yellowing silicone oil on the polyester fabric through a padding method.
The fabric type is polyester filament yarn heavy twist cloth, the gram weight is 395 g/square meter, and the dyeing dye: dispersing black ECO300 and/or deep blue HGL, silicone oil emulsion 120g/L and penetrating agent 1 g/L; after the fabric is dyed, cooling to 80 ℃, discharging liquid, directly adding 0.5g/L glacial acetic acid, adding 2g/L acid reduction cleaning agent, running for 25 minutes, discharging liquid, washing for 5 minutes by cold water, discharging liquid, washing by cold water, pulling out, dehydrating, scutching, and soaking and rolling the finishing liquid.
The fabric type is T/R wool-like, and the gram weight is 230 g/square meter; the dyeing dye is one or more of disperse bright red GS, disperse yellow S-2G, reactive red 3BS and reactive yellow 3RS, the silicone oil emulsion is 60G/L, and the reactive color fixing agent is 15G/L; after the fabric is dyed in a dispersing mode, discharging liquor, 4g/L of sodium hydrosulfite, 1.5g/L of soda ash, 85 ℃ for 20 minutes, washing with water, dyeing activity, dyeing in an active mode, discharging liquor, adding 1g/L of glacial acetic acid into cold water, neutralizing for 10 minutes at 60 ℃, adding 1g/L of soaping agent, washing with water for 30 minutes, drawing out, dehydrating, scutching and soaking and rolling the finishing liquor.
The fabric type is pure polyester single-sided linen, and the gram weight is 180 g/square meter; dyeing dye: disperse black ECT300 and/or disperse blue 2 BLN; 40g/L of silicone oil emulsion, dispersing and dyeing, discharging liquid, 4g/L of sodium hydrosulfite, 2g/L of soda ash and 90 ℃ for 20 minutes, washing with water, adding 0.5g/L of glacial acetic acid for neutralization at 50 ℃, pulling out, dehydrating and scutching, and soaking and rolling the finishing liquid.
The invention has the beneficial effects that:
the invention prepares a novel organosilicon softening agent without affecting color fastness and with low color change by screening different organosilicon raw materials and carrying out synthesis, modification, emulsification and other routes.
Detailed Description
Embodiments of the present invention are described in detail below, as will be appreciated by one of ordinary skill in the art: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents, and all changes that come within the meaning and range of equivalency of the claims are to be embraced within their scope.
The method firstly researches the influence of the molar ratio of different allyl glycidyl ethers to terminal hydrogen-containing silicone oil on the hydrogen conversion rate of the hydrosilylation reaction, and determines the influence of the terminal hydrogen-containing silicone oil with different molecular weights on the application performance of the product after obtaining the optimal molar ratio of the allyl glycidyl ethers to the terminal hydrogen-containing silicone oil.
The basic property determination and application performance test adopted by the invention for the obtained intermediate and the high-fastness ultralow-yellowing silicone oil comprise:
1) and measuring the hydrogen conversion rate of the hydrosilylation reaction in the reaction of the hydrogen-containing polysiloxane at two ends and the allyl glycidyl ether by high performance liquid chromatography.
2) The softness of the fabric is evaluated by a hand touch method to the hand feeling effect of each softener finishing sample, more than five persons are required to evaluate, the highest score is 5 points, the lowest score is 1 point, the sum is the score of the fabric, and the score represents the softness of the fabric.
3) The soaping color fastness is tested according to the soaping color fastness test of GB/T3921 and 2008 textile color fastness test, and the rubbing color fastness is tested according to the rubbing color fastness test of GB/T3920 and 2008 textile color fastness test.
4) Color difference: and testing delta L, delta a, delta b and delta E before and after the fabric is deepened by using a computer color measuring instrument, wherein the delta L is the brightness difference, the delta a is the red-green light difference, the delta b is the yellow-blue light difference, and the delta E is the total color difference. Δ E is calculated by the following equation: Δ E ═ [ (Δ L ·)2+(Δa*)2+(Δb*)2]1/2The larger the value of Δ E, the larger the color difference, and the Δ E at the time of setting off the machine and the Δ E at the time of exposure to air for 30 days were measured, respectively.
Example 1:
(1) adding hydrogen-containing polysiloxane and allyl glycidyl ether at two ends into a four-neck flask with a thermometer according to the molar ratio of 1.8:1, uniformly stirring and heating to 85 ℃, adding 50ppm chloroplatinic acid catalyst (calculated according to the active ingredients of the chloroplatinic acid), uniformly stirring and mixing, heating to 100 ℃, keeping the temperature for 4 hours, and stopping the reaction until the characteristic absorption peak of the Si-H bond disappears. And (3) distilling the synthesized product under reduced pressure to remove excessive allyl glycidyl ether to obtain colorless, clear and transparent linear double-end epoxy group polysiloxane, wherein the hydrogen conversion rate of the hydrosilylation reaction is 72 percent.
(2) Adding epoxy-terminated polydimethylsiloxane and anhydrous piperazine with a quantitative molar ratio and a small molecular weight into a four-neck flask with a thermometer, adding ethanol with the mass of 30% of that of the epoxy-terminated polydimethylsiloxane, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain a colorless, clear and transparent ethanol solution of double-end epoxy-group polydimethylsiloxane with a large molecular weight.
(3) In a four-neck flask with a thermometer, adding a solvent according to a molar ratio of anhydrous piperazine to dimethyl sulfate of 1: 2, adding an ethanol solution of double-end epoxy group polydimethylsiloxane with large molecular weight and dimethyl sulfate, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain the light yellow quaternized polydimethylsiloxane.
(4) 100 g of quaternized modified epoxy-terminated silicone oil and 10g of emulsifier (80 ℃) are added into a plastic beaker at one time, and the plastic beaker is put into a thermostatic water bath at 60 ℃ and is kept warm to 60 ℃. Taking out the plastic beaker, adding about 10g of warm water with the temperature of 60 ℃, and uniformly stirring the materials by using a glass rod. At this time, the viscosity of the material begins to increase slowly, and the system is still in a water-in-oil state; while stirring, about 18g of warm water at 60 ℃ was slowly added by a dropper, one dropper each time. At this time, the viscosity of the material is obviously increased to about 10g, and the viscosity of the material reaches the maximum and then gradually decreases. In this process, the material undergoes a phase inversion process, in particular from water-in-oil to oil-in-water. In the process, water addition cannot be too fast, the next drop of pipe water can be added after the materials are fully stirred after each drop of pipe water is added, if the water addition is too fast, a system does not pass through the highest peak of viscosity, phase inversion is not sufficient, the particle size of the final emulsion is larger or the particle size distribution range is too wide, and the stability of the emulsion and even the application performance of the emulsion are affected; adding a proper amount of water into the system while stirring to ensure that the system has good fluidity, wherein the water adding speed can be relatively high in the process because the material phase inversion is completed, the process is only a thinning process, and the particle size distribution of the emulsion are determined.
And (3) applying the prepared silicone oil emulsion to the fabric by a padding method, and testing the color fastness of washing, the dry-wet rubbing fastness, the color change after cooling off the machine and the color change after standing for 30 days.
Example 2:
the hydrosilylation reaction hydrogen conversion was determined to be 81% by the same procedure as in example 1, except that the hydrogenpolysiloxane and allyl glycidyl ether were added at a 2:1 molar ratio according to example 1.
Example 3:
the hydrogen conversion of the hydrosilylation reaction was found to be 88% by following example 1 by adding a both terminal hydrogenpolysiloxane and allyl glycidyl ether at a molar ratio of 2.2:1 and otherwise proceeding as in example 1.
Example 4:
the hydrogen conversion of the hydrosilylation reaction was measured to be 97.3% by the same procedure as in example 1 except that the hydrogen-containing polysiloxane having both ends and allyl glycidyl ether were added in a molar ratio of 2.4:1 according to example 1.
Example 5:
the hydrogen conversion of the hydrosilylation reaction was measured to be 97.3% by the same procedure as in example 1 except that the hydrogen-containing polysiloxane having both ends and allyl glycidyl ether were added in a molar ratio of 2.5:1 according to example 1.
Example 6:
the hydrogen conversion of the hydrosilylation reaction was determined to be 97.2% by the same procedure as in example 1, except that the hydrogenpolysiloxane and allyl glycidyl ether were added at both ends in a molar ratio of 2.6:1 in accordance with example 1.
In order to obtain high-purity terminal epoxy silicone oil and reduce the residual amount of terminal hydrogen-containing silicone oil in the terminal epoxy silicone oil, the conversion rate of the terminal hydrogen-containing silicone oil needs to be improved as much as possible. For this purpose, an excess of allyl glycidyl ether needs to be added to the system. After the reaction was complete, the excess allyl glycidyl ether was distilled off. As seen in the above examples, when the molar ratio of allyl glycidyl ether to terminal hydrosilicon oil is less than 2.4:1, the hydrogen conversion rate of the hydrosilylation reaction is gradually improved along with the increase of the proportion of the allyl glycidyl ether; when the molar ratio of the allyl glycidyl ether to the terminal hydrogen-containing silicone oil reaches 2.4:1, the hydrogen conversion rate of hydrosilylation reaches the maximum value of 97.3%, the proportion of allyl glycidyl ether is increased, the hydrogen conversion rate of hydrosilylation tends to be constant, and therefore, the molar ratio of the fixed allyl glycidyl ether to the terminal hydrogen-containing silicone oil in the subsequent examples is 2.4: 1.
example 7:
(1) into a four-necked flask with a thermometer, the reaction solution was introduced into a reactor at a molar ratio of 2.4:1 adding hydrogen-containing polysiloxane with molecular weight of 2500 at two ends and allyl glycidyl ether, uniformly stirring, heating to 85 ℃, adding 50ppm chloroplatinic acid catalyst (calculated according to the active ingredients of the chloroplatinic acid), uniformly stirring and mixing, heating to 100 ℃, keeping the temperature for 4 hours, and stopping the reaction until the characteristic absorption peak of the Si-H bond disappears. And removing excessive allyl glycidyl ether after the synthetic product is subjected to reduced pressure distillation to obtain colorless, clear and transparent linear double-end epoxy polysiloxane.
Steps (2), (3) and (4) were the same as in example 1.
Example 8:
(1) according to example 7, the molecular weight of the added hydrogen-containing polysiloxane at both ends was changed to 5000, and the others were not changed.
Steps (2), (3) and (4) were the same as in example 1.
Example 9:
(1) according to example 7, the molecular weight of the added both-terminal hydrogenpolysiloxane was changed to 7000, and the others were unchanged.
Steps (2), (3) and (4) were the same as in example 1.
Example 10:
(1) according to example 7, the molecular weight of the added hydrogen-containing polysiloxane at both ends was changed to 12000, and the others were not changed.
Steps (2), (3) and (4) were the same as in example 1.
The following list 3 examples without thereby limiting the invention to the scope of the embodiments described.
Application example 1:
the fabric types are as follows: the gram weight of the polyester filament yarn hard twisted cloth is 395 g/square meter;
dyeing dye: disperse Black ECO300, disperse dark blue HGL
The dyeing method comprises the following steps: dipping method (high temperature high pressure overflow dyeing machine)
Equipment: a Fuji setting machine (9 sections of oven) of the letter door;
vehicle speed: 15 m/min;
setting temperature: 120 deg.C, 165 deg.C, 180 deg.C, 140 deg.C
Pressure: 3 kg.
The test process comprises the following steps:
120g/L of silicone oil emulsion and 1g/L of penetrant.
After dyeing, cooling to 80 ℃, discharging liquid, directly adding 0.5g/L glacial acetic acid, adding 2g/L acid reduction cleaning agent, running for 25 minutes, discharging liquid, washing for 5 minutes with cold water, discharging liquid, washing with cold water, pulling out, dehydrating, scutching, and soaking and rolling the finishing liquid. Samples were taken for testing the properties, which are shown in tables 1 and 2 below.
Table 1 application example 1 measurement of various performance indexes
Note: the hand feeling evaluation is carried out by five persons, 5 is the highest score, 1 is the lowest score, the total score is obtained by adding, the following is the same
TABLE 2 Wash fastness of application example 1
| Dyeing cloth | Other samples 1 | Other samples 2 | Example 7 | Example 8 | Example 9 | Example 10 | |
| Acetic ester | 3 | 2 | 1-2 | 2-3 | 3 | 3 | 2-3 |
| Cotton | 4 | 2-3 | 2-3 | 4 | 4 | 4 | 3-4 |
| Nylon | 2-3 | 1-2 | 1-2 | 2-3 | 2-3 | 3 | 2-3 |
| Terylene | 3 | 1-2 | 2 | 2-3 | 3 | 3 | 3 |
| Acrylic fibre | 3-4 | 2-3 | 2-3 | 3-4 | 3-4 | 3-4 | 3-4 |
| Wool | 3-4 | 2 | 2 | 3 | 3-4 | 3-4 | 3 |
Application example 2:
the fabric types are as follows: T/R wool-like, the gram weight is 230 g/square meter;
dyeing dye: disperse scarlet GS, disperse yellow S-2G, reactive Red 3BS, reactive yellow 3RS
The dyeing method comprises the following steps: dipping method (high temperature high pressure overflow dyeing machine)
Equipment: a Fuji setting machine (8 sections of oven) of the letter door;
vehicle speed: 25 m/min;
setting temperature: 140 ℃ 175 ℃, 145 ℃ and
pressure: 3.5 kg.
The test process comprises the following steps:
60g/L of silicone oil emulsion and 15g/L of active color fixing agent.
After disperse dyeing is finished, liquid discharging is carried out, 4g/L of sodium hydrosulfite, 1.5g/L of soda ash and 85 ℃ for 20 minutes, after the disperse dyeing is finished, dyeing activity and active dyeing are finished, liquid discharging is carried out, cold water is added into glacial acetic acid and 1g/L of glacial acetic acid and is neutralized for 10 minutes at 60 ℃, soaping agent is added and is 1g/L of the soaping agent and 80 ℃ for 30 minutes, the liquid is washed and pulled out, dewatering and scutching are carried out, finishing liquid is soaked and rolled in one time, and sampling is carried out to test various performances, wherein the performances are shown in the following tables 3 and 4.
Table 3 application example 2 measurement of various performance indexes
TABLE 4 Wash fastness of application example 2
| Dyeing cloth | Other samples 1 | Other samples 2 | Example 7 | Example 8 | Example 9 | Example 10 | |
| Acetic ester | 3 | 2-3 | 1-2 | 2-3 | 3 | 3 | 2-3 |
| Cotton | 3 | 2-3 | 2 | 3 | 3 | 3-4 | 3 |
| Nylon | 3 | 1-2 | 1 | 3 | 3 | 2-3 | 2-3 |
| Terylene | 3 | 1-2 | 2 | 2-3 | 2-3 | 3 | 3 |
| Acrylic fibre | 4 | 2-3 | 2-3 | 4 | 3-4 | 4 | 3-4 |
| Wool | 3 | 2 | 1-2 | 2-3 | 3 | 3 | 3 |
Application example 3:
the fabric types are as follows: pure polyester single-side linen imitation, the gram weight is 180 g/square meter;
dyeing dye: disperse Black ECT300, disperse blue 2BLN
The dyeing method comprises the following steps: dipping method (high temperature high pressure airflow dyeing machine)
Equipment: a Fuji setting machine (8 sections of oven) of the letter door;
vehicle speed: 32 m/min;
setting temperature: 140 ℃ 175 ℃, 145 ℃ and
pressure: 3.5 kg.
The test process comprises the following steps:
the silicone oil emulsion is 40 g/L.
After disperse dyeing is finished, liquid is discharged, sodium hydrosulfite is 4g/L, soda is 2g/L, the temperature is 90 ℃ for 20 minutes, after the sodium hydrosulfite is washed clean, glacial acetic acid is added into the sodium hydrosulfite for neutralization at the temperature of 50 ℃, the sodium hydrosulfite is pulled out, dehydrated and opened, and the finishing liquid is soaked and rolled once. The samples were taken and tested for various properties, which are shown in tables 5 and 6 below.
TABLE 5 application example 3 measurement of various performance indexes
TABLE 6 Wash fastness of application example 3
| Dyeing cloth | Other samples 1 | Other samples 2 | Example 7 | Example 8 | Example 9 | Example 10 | |
| Acetic ester | 3-4 | 2 | 2 | 3 | 3-4 | 3-4 | 3 |
| Cotton | 3-4 | 3 | 2-3 | 3-4 | 4 | 3-4 | 3 |
| Nylon | 3 | 2-3 | 2 | 3 | 2-3 | 3 | 3 |
| Terylene | 3 | 2 | 2 | 2-3 | 2-3 | 3 | 3 |
| Acrylic fibre | 4 | 3 | 2-3 | 3-4 | 3-4 | 4 | 3-4 |
| Wool | 3-4 | 3 | 2-3 | 3 | 3 | 3-4 | 3 |
Claims (3)
1. A polyester fabric is characterized in that: preparing high-fastness ultralow-yellowing silicone oil for the polyester fabric, and performing soaking and rolling on the polyester fabric by using the high-fastness ultralow-yellowing silicone oil for the polyester fabric; the fabric is polyester filament yarn heavy twist cloth, the gram weight is 395 g/square meter, and the dyeing dye: dispersing black ECO300 and/or deep blue HGL, silicone oil emulsion 120g/L and penetrating agent 1 g/L; the padding method comprises the following steps: cooling the fabric to 80 ℃ after dyeing, directly adding 0.5g/L of glacial acetic acid without discharging liquid, adding 2g/L of acidic reduction cleaning agent, running for 25 minutes, discharging liquid, washing for 5 minutes by cold water, discharging liquid, washing by cold water, pulling out, dehydrating and scutching; the preparation method of the high-fastness ultralow-yellowing silicone oil for the polyester fabric comprises the following steps:
1) adding hydrogen-containing polysiloxane and allyl glycidyl ether at two ends into a four-neck flask with a thermometer according to a certain molar ratio, uniformly stirring and heating to 85 ℃, adding 50ppm chloroplatinic acid catalyst, uniformly stirring and mixing, heating to 100 ℃, keeping the temperature for 4 hours, and stopping the reaction until a characteristic absorption peak of a Si-H bond disappears; removing excessive allyl glycidyl ether after the synthetic product is subjected to reduced pressure distillation to obtain colorless, clear and transparent linear double-end epoxy polysiloxane;
2) adding epoxy-terminated polydimethylsiloxane and anhydrous piperazine with a quantitative molar ratio and a small molecular weight into a four-neck flask with a thermometer, adding ethanol with the mass of 30% of that of the epoxy-terminated polydimethylsiloxane, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain a colorless, clear and transparent ethanol solution of double-end epoxy-group polydimethylsiloxane with a large molecular weight;
3) in a four-neck flask with a thermometer, adding a solvent according to a molar ratio of anhydrous piperazine to dimethyl sulfate of 1: 2, adding an ethanol solution of double-end epoxy group polydimethylsiloxane with large molecular weight and dimethyl sulfate, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain light yellow quaternized polydimethylsiloxane;
4) adding 100 g of quaternized modified epoxy-terminated silicone oil and a certain amount of emulsifier into a plastic beaker at one time, putting the plastic beaker into a thermostatic water bath at 60 ℃ and keeping the temperature to 60 ℃, taking out the plastic beaker, adding 10g of 60 ℃ warm water, and uniformly stirring the materials by using a glass rod; while stirring, 18g of 60 ℃ warm water was added slowly by a dropper.
2. A polyester fabric is characterized in that: preparing high-fastness ultralow-yellowing silicone oil for the polyester fabric, and performing soaking and rolling on the polyester fabric by using the high-fastness ultralow-yellowing silicone oil for the polyester fabric; the fabric is T/R wool-like and has the gram weight of 230 g/square meter; the dyeing dye is one or more of disperse bright red GS, disperse yellow S-2G, reactive red 3BS and reactive yellow 3RS, the silicone oil emulsion is 60G/L, and the reactive color fixing agent is 15G/L; the padding method comprises the following steps: after the fabric is dyed in a dispersing way, discharging liquid, wherein 4g/L of sodium hydrosulfite and 1.5g/L of soda are discharged, the temperature is 85 ℃ for 20 minutes, after the fabric is washed clean, dyeing activity is carried out, the dyeing is finished in an active way, discharging liquid, adding cold water into 1g/L of glacial acetic acid and the temperature is 60 ℃ for neutralizing for 10 minutes, adding 1g/L of soaping agent, and the temperature is 80 ℃ for 30 minutes, washing clean and pulling out, and dewatering and scutching; the preparation method of the high-fastness ultralow-yellowing silicone oil for the polyester fabric comprises the following steps:
1) adding hydrogen-containing polysiloxane and allyl glycidyl ether at two ends into a four-neck flask with a thermometer according to a certain molar ratio, uniformly stirring and heating to 85 ℃, adding 50ppm chloroplatinic acid catalyst, uniformly stirring and mixing, heating to 100 ℃, keeping the temperature for 4 hours, and stopping the reaction until a characteristic absorption peak of a Si-H bond disappears; removing excessive allyl glycidyl ether after the synthetic product is subjected to reduced pressure distillation to obtain colorless, clear and transparent linear double-end epoxy polysiloxane;
2) adding epoxy-terminated polydimethylsiloxane and anhydrous piperazine with a quantitative molar ratio and a small molecular weight into a four-neck flask with a thermometer, adding ethanol with the mass of 30% of that of the epoxy-terminated polydimethylsiloxane, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain a colorless, clear and transparent ethanol solution of double-end epoxy-group polydimethylsiloxane with a large molecular weight;
3) in a four-neck flask with a thermometer, adding a solvent according to a molar ratio of anhydrous piperazine to dimethyl sulfate of 1: 2, adding an ethanol solution of double-end epoxy group polydimethylsiloxane with large molecular weight and dimethyl sulfate, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain light yellow quaternized polydimethylsiloxane;
4) adding 100 g of quaternized modified epoxy-terminated silicone oil and a certain amount of emulsifier into a plastic beaker at one time, putting the plastic beaker into a thermostatic water bath at 60 ℃ and keeping the temperature to 60 ℃, taking out the plastic beaker, adding 10g of 60 ℃ warm water, and uniformly stirring the materials by using a glass rod; while stirring, 18g of 60 ℃ warm water was added slowly by a dropper.
3. A polyester fabric is characterized in that: preparing high-fastness ultralow-yellowing silicone oil for the polyester fabric, and performing soaking and rolling on the polyester fabric by using the high-fastness ultralow-yellowing silicone oil for the polyester fabric; the fabric is pure polyester single-sided linen-like, and the gram weight is 180 g/square meter; dyeing dye: dispersing black ECT300 and/or dispersing blue 2BLN, and silicone oil emulsion 40g/L, wherein the padding method comprises the following steps: after the disperse dyeing is finished, discharging liquor, namely 4g/L of sodium hydrosulfite and 2g/L of soda ash, washing the liquor for 20 minutes at 90 ℃, adding 0.5g/L of glacial acetic acid for neutralization at 50 ℃, pulling out, dehydrating and scutching; the preparation method of the high-fastness ultralow-yellowing silicone oil for the polyester fabric comprises the following steps:
1) adding hydrogen-containing polysiloxane and allyl glycidyl ether at two ends into a four-neck flask with a thermometer according to a certain molar ratio, uniformly stirring and heating to 85 ℃, adding 50ppm chloroplatinic acid catalyst, uniformly stirring and mixing, heating to 100 ℃, keeping the temperature for 4 hours, and stopping the reaction until a characteristic absorption peak of a Si-H bond disappears; removing excessive allyl glycidyl ether after the synthetic product is subjected to reduced pressure distillation to obtain colorless, clear and transparent linear double-end epoxy polysiloxane;
2) adding epoxy-terminated polydimethylsiloxane and anhydrous piperazine with a quantitative molar ratio and a small molecular weight into a four-neck flask with a thermometer, adding ethanol with the mass of 30% of that of the epoxy-terminated polydimethylsiloxane, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain a colorless, clear and transparent ethanol solution of double-end epoxy-group polydimethylsiloxane with a large molecular weight;
3) in a four-neck flask with a thermometer, adding a solvent according to a molar ratio of anhydrous piperazine to dimethyl sulfate of 1: 2, adding an ethanol solution of double-end epoxy group polydimethylsiloxane with large molecular weight and dimethyl sulfate, uniformly stirring, heating to 78-80 ℃, and keeping the temperature for 14 hours to obtain light yellow quaternized polydimethylsiloxane;
4) adding 100 g of quaternized modified epoxy-terminated silicone oil and a certain amount of emulsifier into a plastic beaker at one time, putting the plastic beaker into a thermostatic water bath at 60 ℃ and keeping the temperature to 60 ℃, taking out the plastic beaker, adding 10g of 60 ℃ warm water, and uniformly stirring the materials by using a glass rod; while stirring, 18g of 60 ℃ warm water was added slowly by a dropper.
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| CN1735648A (en) * | 2002-11-04 | 2006-02-15 | Ge拜尔硅股份有限公司 | Linear polyamino and/or polyammonium polysiloxane copolymers I |
| CN102558567A (en) * | 2011-12-10 | 2012-07-11 | 江阴市尼美达助剂有限公司 | Preparation method of quaternary copolymer block organic silicon oil |
| GB201216638D0 (en) * | 2012-09-18 | 2012-10-31 | Devan Chemicals Nv | textile treatment compounds and compositions |
| CN104761723A (en) * | 2015-04-09 | 2015-07-08 | 南丰县大信科技有限公司 | Polysiloxane softening agent with color fixing property |
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| CN1735648A (en) * | 2002-11-04 | 2006-02-15 | Ge拜尔硅股份有限公司 | Linear polyamino and/or polyammonium polysiloxane copolymers I |
| CN102558567A (en) * | 2011-12-10 | 2012-07-11 | 江阴市尼美达助剂有限公司 | Preparation method of quaternary copolymer block organic silicon oil |
| GB201216638D0 (en) * | 2012-09-18 | 2012-10-31 | Devan Chemicals Nv | textile treatment compounds and compositions |
| CN104761723A (en) * | 2015-04-09 | 2015-07-08 | 南丰县大信科技有限公司 | Polysiloxane softening agent with color fixing property |
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