CN110437460A - A kind of synthesis technology of anion-modified hyperbranched silicone softening agent and its dyeing of fabric - Google Patents
A kind of synthesis technology of anion-modified hyperbranched silicone softening agent and its dyeing of fabric Download PDFInfo
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- CN110437460A CN110437460A CN201910707983.5A CN201910707983A CN110437460A CN 110437460 A CN110437460 A CN 110437460A CN 201910707983 A CN201910707983 A CN 201910707983A CN 110437460 A CN110437460 A CN 110437460A
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- 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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- D06P1/38—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 reactive dyes
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- 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
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- 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
- D06P1/673—Inorganic compounds
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- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
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Abstract
The invention discloses a kind of synthesis technology of anion-modified hyperbranched silicone softening agent and its dyeings of fabric.The defects such as scratch, the wrinkle that the anion-modified hyperbranched silicone softening agent that the present invention uses can avoid fabric from generating in dyeing course with textile dyeing with bath, fabric can also be made to be achieved with soft effect in dyeing simultaneously while there is hydrophily, do not need to carry out soft post-processing again after dyeing.
Description
Technical field
The invention belongs to textile dyeing fields, and in particular to a kind of synthesis of anion-modified hyperbranched silicone softening agent
The dyeing of technique and its fabric.
Background technique
The soft finish of fabric is made to reduce between fiber and fiber there are also the frictional resistance between fiber and human body
Obtain a kind of finishing technique that fabric generates soft effect.By the fabric of soft finish, generally can all there be fabulous soft feel,
Softening agent is the chemical assistant for improving fabric feel, and development process experienced grease, surfactant, organosilicon three
In a stage, there are also extremely soft main chains due to there is a physiological inertia that necessity as outstanding softening agent is provided with by it for organosilicon
Condition.
Organic silicon softening agent is increasingly taken seriously due to its unique surface property and excellent softness.State
Fabric after interior majority silicone softening agent arranges is in hydrophobicity, feels sultry when wearing, and be difficult to wash.Many products are also
Often there is demulsification floating oil phenomenon.Though and the hydrophilic polyethers silicone softening agent of tradition has preferable hydrophily and water-soluble
Property, but flexibility and finishing effect durability are poor.Therefore developing has the novel hydrophilic organic of excellent flexibility and durability
Silicone softener has very real meaning.
It is arranged and the problems in manufacturing process to solve over softening agent, various countries develop a variety of organic modified silicas oxygen
Alkane, modified organic group can be introduced into polysiloxane chain by the methods of monomer synthesis, block copolymerization.These active groups
Introducing it is modified greatly improve flexibility, silk slip, water-wash resistance of fabric etc., different groups assigns fabric different characteristics
The multifunctional development that fabric has been adapted to the arrangement such softening agent of style, assigns fabric hydrophilic, flexibility, pilling resistance
Etc. performances while so that the excellent performance of the script of fabric does not change, these modified silicon oils be can be used alone,
Can also be used in mixed way, by the processed fabric of these modified silicon oils, produce better feel and wash durability also very
It is good.
It is the most excellent with anion-modified polysiloxanes in various modified siloxane softening agents, however by synthetic method,
The limitation of raw material, emulsifier and emulsification condition, structure have very big difference, and at the same time, people are to anion-modified silicone oil
Requirement increasingly improve, select suitable amino silicon oil emulsion and technique applied to fabric critically important.
In the competition of various softening agents, excellent flexibility depends on its basic geometrical molecular configuration, due to
The silicon oxygen chain structure of polysiloxanes has very big bond angle and bond distance, and oxygen atom and silicon atom are easy to distortion composition spiral straight chain
Type structure, then two organic groups rotate around silicon oxygen bond on each silicon atom, can freely revolve around 360 ° of main chain
Turn, so main chain has reached submissive effect, this just determines that polysiloxanes can become the good softening agent of fabric.It is same with this
When, the spatial volume of organic group on main chain is very big, energy very little required for rotating, so permeability is good.Polysiloxanes
Molecule between spacing it is very big because intermolecular active force is smaller, viscosity is lower, and surface tension is smaller, and filming performance is strong,
It is adsorbed in the organosilicon macromolecule film forming of fabric surface, elastic net structure is generated, not only maintains good softness in this way
Effect, while being also provided with good water-wash resistance.
Summary of the invention
Goal of the invention: in order to solve the deficiencies in the prior art, the present invention provides a kind of anion-modified hyperbranched organic
The synthesis technology of silicone softener and its dyeing of fabric.
Technical solution: a kind of synthesis technology of anion-modified hyperbranched silicone softening agent, concrete operations are as follows:
Anion-modified hyperbranched silicone softening agent is that there are also amine-terminated hyperbrancedization polysiloxanes as raw material using sodium chloroacetate
Graft reaction is carried out, is made to 250mL with the isopropanol that a certain amount of hyperbranched silicone and 30% are added in the flask of condenser pipe
For solvent, then a certain amount of sodium chloroacetate is dissolved with distilled water, open simultaneously condensed water cooling, starts that chloroethene is at the uniform velocity added dropwise
Acid sodium solution controls temperature and charging rate, sufficiently reacts 4 hours at 80 DEG C of temperature after being added dropwise, and adjusts pH value in 11-
Between 12, a kind of product that can dye same bath is finally obtained, will be obtained after obtained oily transparent products distillation water emulsification
The anion-modified hyperbranched silicone softening agent of finishing agent required for experiment.
A kind of reactive dye that the synthesis technology of the anion-modified hyperbranched silicone softening agent according to is prepared
The production technology of upper dye pure cotton fabric, concrete operations are as follows:
Preparing 5 pieces of cotton mercerising bleaching semi-products, specification 20*10cm calculates dye liquor total amount according to the bath raio of 1:20, according still further to
5g/L, which is incremented by, to be weighed 5 anion-modified hyperbranched silicone softening agents from 0-20g/L and is added separately to 250ml beaker in order
It is interior, it is stand-by to be prepared into dyestuff according still further to 4% o.w.f of reactive brilliant red 3BSN, sodium chloride 20g/L, sodium carbonate 15g/L；
Dyestuff is added in sequence in beaker and adds water to each dye bath total amount, then beaker is put into thermostat water bath and is heated to
It after 60 DEG C, puts into dye liquor after being extracted after fabric is soaked with water, stirs one by one, after dyeing 10min, pick up fabric and chlorine is added
Change sodium, fabric is put back to after stirring and dissolving, continue dye after ten minutes, picks up fabric and sodium carbonate is added, fabric is put after stirring and dissolving
It returns, water bath temperature is adjusted to 90 DEG C, fixation 30min is kept stirring in dyeing course at 90 DEG C, in liquid level
Place marks, and interruption supplement hot water maintains dye bath bath raio；Dyeing residual liquid is toppled over after the completion of dyeing, is first washed with cold water, then
Soap 10min under conditions of 95 DEG C, and then hot water wash-cold water takes out article after wash-drying again.
A kind of disperse dyes that the synthesis technology of the anion-modified hyperbranched silicone softening agent according to is prepared
The production technology of upper dye dacron, concrete operations are as follows:
Prepare 5 pieces of terylene bleaching semi-products, specification 20*10cm calculates dye liquor total amount according to the bath raio of 1:20, according still further to 5g/L
It is incremented by from 0-20g/L and weighs 5 anion-modified hyperbranched silicone softening agents, claims according still further to the dosage of 2% o.w.f of disperse yellow
Disperse dyes are taken to be added separately in 150mL dye model machine Dyeing pipe in order；
After disperse dye solutions at 40 DEG C are shaken up, with the acetum diluted adjust the dyestuff pH value in each Dyeing pipe to
6, it extracts, is put into dye liquor after then soaking fabric with water, Dyeing pipe is fitted into dye model machine, starting dye model machine, dye
Liquid is warming up to 130 DEG C of poststaining 30min, after cooling down, takes out fabric, is first washed with cold water, then carry out reduction cleaning, temperature is
85 DEG C, time 10min, bath raio 50:1, article is taken out in drying after cold water washes.
The utility model has the advantages that hyperbranched silicone softening agent has a variety of end groups, and reactivity is high, can use to it
Terminal groups modification, to realize the functionalization of hyperbranched silicone softening agent, the present invention is used anion-modified hyperbranched organic
The defects such as scratch, the wrinkle that silicone softener can avoid fabric from generating in dyeing course with textile dyeing with bath, simultaneously
Fabric can also be made to be achieved with soft effect in dyeing while there is hydrophily, do not need to carry out softness again after dyeing
Post-processing.
The present invention probes into two kinds of colouring methods using control variate method --- and reactive dye contaminate pure cotton fabric, disperse dyes dye
Influence of the concentration of dacron different softening agents under same dyeing condition to dyeing effect, and how to control single dyeing strip
Part makes dyeing effect more preferable and fabric has good softness.
There are also amine-terminated hyperbrancedization polyethers amino block polysiloxanes as Material synthesis one using sodium chloroacetate by the present invention
The novel anion-modified hyperbranched silicone softening agent of finishing agent of kind, the dyeing course applied to cotton fabric and dacron
In, influence of the concentration of different anions modified ultra-branching silicone softening agent to dyeing effect is discussed respectively, is then optimized
Dyeing condition, so that anion-modified hyperbranched silicone softer consistency bring discoloration in dyeing course, on
Dye rate reduce and hydrophily reduce flaw removed so that fabric not only obtained in dyeing course it is good soft
Soft energy, also improves the dye-uptake of dyestuff, has obtained conclusion below:
When dyeing cotton fabric on reactive dye, when the concentration of anion-modified hyperbranched silicone softening agent is added less than 10g/L,
The softness of cotton fabric is improved, so that scratch is avoided in dyeing course, the defects such as fold, and at the same time, although
Anion-modified hyperbranched silicone softening agent adheres in fabric surface to form a film, but the dyeing ability of dyestuff does not cause shadow
It rings, when the concentration of anion-modified hyperbranched silicone softening agent is greater than 10g/L, with anion-modified hyperbranched silicone
The dyeing ability of the raising of softer consistency, dyestuff is substantially reduced.
When contaminating dacron on disperse dyes, the concentration of the anion-modified hyperbranched silicone softening agent of addition is less than
When 10g/L, the softness of dacron is improved, so that scratch is avoided in dyeing course, the defects such as fold, with this
Meanwhile forming a film although anion-modified hyperbranched silicone softening agent adheres in fabric surface, the dyeing ability of dyestuff does not have
It impacts, when the concentration of anion-modified hyperbranched silicone softening agent is greater than 10g/L, with anion-modified over-expense
Change the raising of silicone softening agent concentration, the dyeing ability of dyestuff is substantially reduced.
Detailed description of the invention
Fig. 1 is the process of grafting schematic diagram of hyperbranched silicone of the invention；
Fig. 2 is reactive dyeing process curve synoptic diagram of the invention；
Fig. 3 is disperse dyeing process curve synoptic diagram of the invention.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, so that the technology of this field
Personnel can better understand advantages and features of the invention, to make apparent boundary to protection scope of the present invention
It is fixed.Embodiment described in the invention is only a part of the embodiment of the present invention, instead of all the embodiments, based on the present invention
In embodiment, those of ordinary skill in the art's every other implementation obtained without making creative work
Example, shall fall within the protection scope of the present invention.
Embodiment
1. the synthesis of anion-modified hyperbranched silicone softening agent
Anion-modified hyperbranched silicone softening agent is that there are also amine-terminated hyperbrancedization polysiloxanes as raw material using sodium chloroacetate
Graft reaction is carried out, is made to 250mL with the isopropanol that a certain amount of hyperbranched silicone and 30% are added in the flask of condenser pipe
For solvent.Then a certain amount of sodium chloroacetate is dissolved with distilled water, opens simultaneously condensed water cooling, start that chloroethene is at the uniform velocity added dropwise
Acid sodium solution controls temperature and charging rate, sufficiently reacts 4 hours under conditions of 80 DEG C of temperature after being added dropwise, and adjusts pH
Value finally obtains a kind of product (reaction process is as shown in Figure 1) that can dye same bath, the oily that will be obtained between 11-12
The anion-modified hyperbranched silicone softening agent of finishing agent required for being tested after transparent products distillation water emulsification.
2. contaminating pure cotton fabric on reactive dye
Operating procedure is as follows:
Prepare 5 pieces of cotton mercerising bleachings semi-products (specification 20*10cm), calculates dye liquor total amount according to the bath raio of 1:20, according still further to
5g/L, which is incremented by, to be weighed 5 anion-modified hyperbranched silicone softening agents from 0-20g/L and is added separately to 250ml beaker in order
It is interior, according still further to reactive brilliant red 3BSN 4%(o.w.f), it is spare to weigh experimental drug by sodium chloride 20g/L, sodium carbonate 15g/L.
The dyestuff weighed up is added in sequence in beaker and adds water to each dye bath total amount, then puts beaker into thermostatted water
Bath is put into dye liquor after extracting after soaking fabric with water after being heated to 60 DEG C, is stirred one by one, after dyeing 10min, is picked up
Sodium chloride is added by tabular sequence in fabric, and fabric is put back to after stirring and dissolving, continues dye after ten minutes, fabric is picked up, according to table
Sodium carbonate is added in sequence, and fabric is put back to after stirring and dissolving, water bath temperature is adjusted to 90 DEG C, fixation 30min, In at 90 DEG C
In dyeing course, it is kept stirring.It is marked in the place of liquid level, interruption supplement hot water maintains dye bath bath raio.
Dyeing residual liquid is toppled over after the completion of dyeing, is first washed with cold water, then soap under conditions of 95 DEG C 10min, then again
Taking-up fabric is to be measured after hot water wash-cold water wash-is dried, process curve such as Fig. 2.
3. contaminating dacron on disperse dyes
Operating procedure is as follows:
Prepare 5 pieces of terylene bleachings semi-products (specification 20*10cm), dye liquor total amount is calculated according to the bath raio of 1:20, according still further to 5g/L
It is incremented by from 0-20g/L and weighs 5 anion-modified hyperbranched silicone softening agents, according still further to the dosage of disperse yellow 2%(o.w.f)
Disperse dyes are weighed to be added separately in order in 150mL dye model machine Dyeing pipe.
After disperse dye solutions are shaken up, the dyestuff pH value in each Dyeing pipe is adjusted to 6 with the acetum diluted, then will
Fabric is extracted after being soaked with water, is put into dye liquor, and Dyeing pipe is packed into dye model machine.It is compiled according to the process curve of Fig. 3
After journey starting dye model machine dyeing program, after cooling down, take out fabric, first washed with cold water, then carry out reduction cleaning (85 DEG C,
10min, bath raio 50:1), it is to be measured to take out fabric for drying after cold water washes.
4. test and characterization
4.1 fabric apparent colour depth
Using the apparent colour depth (K/S value) of DatacolorSF650 color measurement and color match instrument measurement dyed fabric, K/S value is bigger
I.e. upper dye effect is better, and the smaller i.e. anion-modified hyperbranched silicone softening agent of K/S is to being infected with blocking effect on dyestuff.
The test of 4.2 pliabilitys
(1) using the flexibility of fabric after the measurement dyeing of FAST-2 Fabric Style instrument, when the bending stiffness of fabric is smaller, fabric
Softness it is better.Fabric after dyeing is cut into the sample of 5x13cm specification, is then lain in a horizontal plane in measurement plane,
Fabric is covered with pressure plare and leaks out 5mm by natural selvedge, is then slowly pushed forward, sample one end leaves level table cloth specimen and is in
It is cantilever-shaped, it is bent to when being in contact with 45 ° of inclined-planes instantly, blocks illumination, the green light on instrument becomes red light, and record stretches out water at this time
The sample length of flat surface, is denoted as bending length, and length gets over that section i.e. rigidity is smaller, and the softness of fabric is better.
(2) touch grading is carried out to fabric using 5 people grading method simultaneously.Feel grade is divided into 5 grades, 5 grades preferably, not
The blank sample of arrangement is 1 grade.
The measurement of 4.3 dye-uptakes
With V-1200 type visible spectrophotometer, the absorbance of dye liquor before and after the measurement dyeing of maximum absorption wave strong point, according to
Formula calculates dye-uptake:
In formula: A0To dye the absorbance after preceding dye liquor dilutes m times
A1Absorbance after diluting n times for dye liquor after dyeing
The test of 4.4 working solution stability
After dye liquor after various dyeings is stood 24H, check whether phenomena such as floating oil, layering occur, and keep a record.
5. influence of the anion-modified hyperbranched silicone softening agent dosage to fabric K/S value
It will be by anion-modified hyperbranched silicone softening agent dyeing cotton fabric and the dispersion on reactive dye respectively of technique production
Co-bathing dyeing is carried out to fabric when contaminating dacron on dyestuff, observes anion-modified hyperbranched silicone softening agent mass concentration
Influence to fabric K/S value the results are shown in Table 1:
Influence of the concentration of the anion-modified hyperbranched silicone softening agent of table 1 to fabric K/S
| Anion-modified hyperbranched silicone softening agent (g/L) | Cotton fabric K/S value | Dacron K/S value |
| 0 | 5.0837 | 26.0280 |
| 5 | 5.9229 | 27.0440 |
| 10 | 6.0277 | 27.3960 |
| 15 | 2.1847 | 25.1070 |
| 20 | 1.3246 | 21.3748 |
Seen from table 1, the K/S value of two kinds of fabrics is equally all the quality with anion-modified hyperbranched silicone softening agent
Concentration is gradually reduced after increasing to 10g/L, this is because it is total with dyestuff just to have started anion-modified hyperbranched silicone softening agent
Same-action increases the K/S of fabric in fabric surface, but with anion-modified hyperbranched
The increase of silicone softening agent mass concentration, the dendrimer in anion-modified hyperbranched silicone softening agent is in fabric
Surface spreading film forming, prevent dyestuff is from being adsorbed on fabric surface completely, so to the effect for having dyed blocking so that
The K/S value of fabric is gradually reduced.
6. influence of the anion-modified hyperbranched silicone softening agent dosage to fabric softness
The fabric after dyeing is tested according to test method, test result such as table 2:
Influence of the concentration of the anion-modified hyperbranched silicone softening agent of table 2 to fabric softness
| Anion-modified hyperbranched silicone softening agent (g/L) | Cotton fabric bending length (mm) | Dacron bending length (mm) | Cotton fabric feel (grade) | Dacron feel (grade) |
| 0 | 20 | 13.5 | 1 | 1 |
| 5 | 17.5 | 12 | 3 | 2 |
| 10 | 16 | 10 | 4 | 4 |
| 15 | 15.5 | 9.5 | 4 | 4 |
| 20 | 15 | 9.5 | 5 | 5 |
As shown in Table 2, when the mass concentration of anion-modified hyperbranched silicone softening agent increases, the bending of two kinds of fabrics
Length is being incrementally decreased, and illustrates fabric in dyeing course due to the quality of anion-modified hyperbranched silicone softening agent
Concentration increases and becomes more and more soft, at the same time, in terms of the feel of fabric for, it is anion-modified hyperbranched in addition
After silicone softening agent softening agent, the feel of fabric can obviously become soft, but when mass concentration is greater than 10g/L, fabric
Feel with softening agent concentration variation and it is alternatively unobvious, this is because anion-modified hyperbranched silicone softening agent
Dissaving structure present it is tree-shaped, have good mobility and film forming, when mass concentration be less than 10g/L when, anion
Modified ultra-branching silicone softening agent incompletely sprawls film forming, so having certain flexibility, when mass concentration is greater than
When 10g/L, the dendrimer in anion-modified hyperbranched silicone softening agent spreads over fabric surface and film forming completely,
Although more soft, soft effect promotion is not very big.
7. influence of the fixation time to fabric K/S value
According to result of study, one group of experiment is designed, by controlling variable, so that the anion-modified hyperbranched silicone being added
The mass concentration of softening agent is 10g/L, other experiment conditions are constant, enables fixation time 30min become variable and studies the fixation time
Influence to K/S value is shown in Table 3:
Influence of the 3 fixation time of table to fabric K/S value
| The fixation time (min) | Cotton fabric K/S value | Dacron K/S value |
| 30 | 6.0356 | 26.9281 |
| 45 | 6.4829 | 27.6440 |
| 60 | 7.1204 | 27.7967 |
| 75 | 7.2596 | 27.8213 |
| 90 | 7.3246 | 27.8448 |
Seen from table 3, by controlling this variable of fixation time, other dyeing conditions and anion-modified hyperbranched silicone
When softening agent mass concentration is consistent, the K/S value of fabric increases with the increase of fixation time, but works as and contaminate cotton on reactive dye
The fabric fixation time reaches 60min and is further added by the fixation time when the right dacron fixation time reaches 45min on disperse dyes
Influence to K/S value is little, this should be because while that fabric surface has had membranaceous macromolecular covering, with the fixation time
Increase, dyestuff gradually penetrates into the hole between fabric fibre, but when the fixation time reaching 60min, fabric is to dyestuff
Degree of absorption reach nearly saturation state, the K/S value of fabric is not had much influence yet so being further added by the fixation time.
8. influence of the dye liquor pH value to dacron K/S value during disperse dyeing
According to result of study, one group of experiment is designed, by controlling variable, so that the anion-modified hyperbranched silicone being added
The mass concentration of softening agent is 10g/L, other experiment conditions are constant, and the pH value of dye liquor is enabled to become variable research pH value to fabric
The influence of K/S value such as table 4:
Influence of 4 dye liquor pH value of table to dacron K/S value
| PH value | K/S value |
| 6 | 25.3783 |
| 7 | 26.2648 |
| 8 | 28.1400 |
| 9 | 20.2607 |
| 10 | 13.6859 |
By table 4 as it can be seen that passing through this variable of the pH value of dye liquor, other dyeing conditions and yin during control disperse dyeing
When ion modification hyperbranched silicone softening agent mass concentration is consistent, the K/S value of fabric first increases with increasing for dye liquor pH value
Reduce after big, illustrate when pH value in alkalescent and more preferable under dye is than solutions of weak acidity on dyestuff when less than 8, this is because adjusting
When pH value, saponification is had occurred in the alkaline agent of addition and anion-modified hyperbranched silicone softening agent, so that anion-modified
Hyperbranched silicone softening agent will not overlay on fabric surface but penetrate into inside fabric fibre, but when the alkaline agent being added
When quantitative change makes pH value be greater than 8 more, alkaline agent is reacted with dyestuff, so that the color of dyestuff is changed, so that fabric
The change dramatically of K/S value.
9. influence of the acetic acid to cotton fabric K/S value is added dropwise in Dyeing with Reactive Dyes
The acetum of 20g/L is prepared, dyeing condition and anion-modified hyperbranched silicone softening agent mass concentration phase are controlled
Together, one group of experiment is designed, after reactive dyeing fixation, the acetum of inequality is separately added into, studies the K/S to fabric
The influence of value such as the following table 5:
Influence of the dropwise addition of 5 acetum of table to cotton fabric K/S value
| Acetum (mL) | K/S value |
| 0 | 6.0178 |
| 2 | 6.2347 |
| 4 | 6.3916 |
| 6 | 6.8843 |
| 8 | 7.1243 |
As shown in Table 5, when gradually dripping acetum, the K/S value of fabric is gradually increased, illustrate the dyeing effect of fabric with
The dropwise addition of acetum and gradually improve, this is because after reactive dye color fixing, anion-modified hyperbranched silicone is soft
Dendrimer in agent is covered on fabric surface, forms blocking effect, and the hydrogen ion in acetum with it is anion-modified
- COO in hyperbranched silicone softening agent-Reaction generates hydrophilic radical-COOH, so that anion-modified hyperbranched silicone
Softening agent hydrophilicity reduces, so that dyestuff be made to be easier to be attached to fabric surface.
10. influence of the different condition to the dye-uptake of dyestuff
Table 6,7,8,9 can be obtained according to the dye-uptake that measuring method calculates dyestuff under different condition.
Dyestuff dye-uptake under 6 different anions modified ultra-branching silicone softening agent concentration of table
| Anion-modified hyperbranched silicone softer consistency (g/L) | Reactive dye dye-uptake (%) | Disperse dyes dye-uptake (%) |
| 0 | 51.3 | 56.8 |
| 5 | 59.5 | 65.2 |
| 10 | 62.3 | 62.1 |
| 15 | 38.7 | 43.1 |
| 20 | 26.4 | 21.3 |
Dyestuff dye-uptake under the different fixation times of table 7
| The fixation time (min) | Reactive dye dye-uptake (%) | Disperse dyes dye-uptake (%) |
| 30 | 61.4 | 64.8 |
| 45 | 63.8 | 67.4 |
| 60 | 66.3 | 67.8 |
| 75 | 66.8 | 68.1 |
| 90 | 66.9 | 68.1 |
The dye-uptake of disperse dyes under the different pH value of table 8
| PH value | Disperse dyes dye-uptake (%) |
| 6 | 63.2 |
| 7 | 66.8 |
| 8 | 64.3 |
| 9 | 33.6 |
| 10 | 18.3 |
Influence of the acetum to contaminating on reactive dye is added dropwise in table 9
| Acetum (mL) | Reactive dye dye-uptake (%) |
| 0 | 60.3 |
| 2 | 66.7 |
| 4 | 68.6 |
| 6 | 69.4 |
| 8 | 69.9 |
According to table 6,7,8,9 it is found that while Optimizing Technical, the dye-uptake of dyestuff becomes with the polarization of condition
Change, so that it is determined that having gone out optimal dyeing condition, so that the softness of fabric and the dyeing ability of dyestuff reach most
It is good, the difficulty performance of dyeing will not be excessively increased again, such as in the dyeing course of cotton fabric, although increasing fixation
The the time the long more the dye-uptake of dyestuff can be made to increase, but when the fixation time reaching 60min, dye-uptake increasing degree compared with
It is small, if continuing growing the fixation time, income very little, however kept for 90 DEG C and need to expend mass energy, so dye-uptake is flat again
It is 60min that the best fixation time is obtained when gradualization, and the best fixation time of dacron is 45min, in 45min fixation
Between after the effect that is characterized and cotton fabric fixation time be consistent after 60min.In two kinds of dyeing courses, yin
Influence of the concentration of ion modification hyperbranched silicone softening agent to the dye-uptake of dyestuff is consistent, in anion-modified over-expense
When the concentration for changing silicone softening agent is 10g/L, the dye-uptake of dyestuff reaches maximum value, continues growing anion-modified hyperbranched
The concentration of silicone softening agent can only make the dye-uptake of dyestuff reduce, because organosilicone film is covered in fabric surface, so that
Dyestuff can not continue to go in upper dye to fabric, to play certain blocking effect.
11. the stability of working solution
After working solution in experiment is stood 24H, after observation it is found that in 1#-10# working solution, 1# and 6# do not add anion to change
Property hyperbranched silicone softening agent, working solution is transparent, and remaining working solution is due to being added the anion-modified super of inequality
There is slight suspension in branched silicone softening agent, has a little attachment on wall of cup, color is in dye colour, however not shadow
Phenomena such as oil spill is layered does not occur for the stability for ringing working solution, it can be seen that the anion-modified hyperbranched silicone softening agent
With good high temperature resistant Dian weak acid resistant and resistance to alkalescent, and under corresponding condition, the same bath of dyeing can be such that fabric has well
Softness.
There are also amine-terminated hyperbrancedization polyethers amino block polysiloxanes as Material synthesis one using sodium chloroacetate by the present invention
The novel anion-modified hyperbranched silicone softening agent of finishing agent of kind, the dyeing course applied to cotton fabric and dacron
In, influence of the concentration of different anions modified ultra-branching silicone softening agent to dyeing effect is discussed respectively, is then optimized
Dyeing condition, so that anion-modified hyperbranched silicone softer consistency bring discoloration in dyeing course, on
Dye rate reduce and hydrophily reduce flaw removed so that fabric not only obtained in dyeing course it is good soft
Soft energy, also improves the dye-uptake of dyestuff, has obtained conclusion below:
When dyeing cotton fabric on reactive dye, when the concentration of anion-modified hyperbranched silicone softening agent is added less than 10g/L,
The softness of cotton fabric is improved, so that scratch is avoided in dyeing course, the defects such as fold, and at the same time, although
Anion-modified hyperbranched silicone softening agent adheres in fabric surface to form a film, but the dyeing ability of dyestuff does not cause shadow
It rings, when the concentration of anion-modified hyperbranched silicone softening agent is greater than 10g/L, with anion-modified hyperbranched silicone
The dyeing ability of the raising of softer consistency, dyestuff is substantially reduced.
When contaminating dacron on disperse dyes, the concentration of the anion-modified hyperbranched silicone softening agent of addition is less than
When 10g/L, the softness of dacron is improved, so that scratch is avoided in dyeing course, the defects such as fold, with this
Meanwhile forming a film although anion-modified hyperbranched silicone softening agent adheres in fabric surface, the dyeing ability of dyestuff does not have
It impacts, when the concentration of anion-modified hyperbranched silicone softening agent is greater than 10g/L, with anion-modified over-expense
Change the raising of silicone softening agent concentration, the dyeing ability of dyestuff is substantially reduced.
Claims (3)
1. a kind of synthesis technology of anion-modified hyperbranched silicone softening agent, it is characterised in that: concrete operations are as follows:
Anion-modified hyperbranched silicone softening agent is that there are also amine-terminated hyperbrancedization polysiloxanes as raw material using sodium chloroacetate
Graft reaction is carried out, is made to 250mL with the isopropanol that a certain amount of hyperbranched silicone and 30% are added in the flask of condenser pipe
For solvent, then a certain amount of sodium chloroacetate is dissolved with distilled water, open simultaneously condensed water cooling, starts that chloroethene is at the uniform velocity added dropwise
Acid sodium solution controls temperature and charging rate, sufficiently reacts 4 hours at 80 DEG C of temperature after being added dropwise, and adjusts pH value in 11-
Between 12, a kind of product that can dye same bath is finally obtained, will be obtained after obtained oily transparent products distillation water emulsification
The anion-modified hyperbranched silicone softening agent of finishing agent required for experiment.
2. a kind of work that the synthesis technology of anion-modified hyperbranched silicone softening agent according to claim 1 is prepared
Property dyestuff on contaminate pure cotton fabric production technology, it is characterised in that: concrete operations are as follows:
Preparing 5 pieces of cotton mercerising bleaching semi-products, specification 20*10cm calculates dye liquor total amount according to the bath raio of 1:20, according still further to
5g/L, which is incremented by, to be weighed 5 anion-modified hyperbranched silicone softening agents from 0-20g/L and is added separately to 250ml beaker in order
It is interior, it is stand-by to be prepared into dyestuff according still further to 4% o.w.f of reactive brilliant red 3BSN, sodium chloride 20g/L, sodium carbonate 15g/L；
Dyestuff is added in sequence in beaker and adds water to each dye bath total amount, then beaker is put into thermostat water bath and is heated to
It after 60 DEG C, puts into dye liquor after being extracted after fabric is soaked with water, stirs one by one, after dyeing 10min, pick up fabric and chlorine is added
Change sodium, fabric is put back to after stirring and dissolving, continue dye after ten minutes, picks up fabric and sodium carbonate is added, fabric is put after stirring and dissolving
It returns, water bath temperature is adjusted to 90 DEG C, fixation 30min is kept stirring in dyeing course at 90 DEG C, in liquid level
Place marks, and interruption supplement hot water maintains dye bath bath raio；Dyeing residual liquid is toppled over after the completion of dyeing, is first washed with cold water, then
Soap 10min under conditions of 95 DEG C, and then hot water wash-cold water takes out article after wash-drying again.
3. a kind of point that the synthesis technology of anion-modified hyperbranched silicone softening agent according to claim 1 is prepared
Dissipate the production technology that dacron is contaminated on dyestuff, it is characterised in that: concrete operations are as follows:
Prepare 5 pieces of terylene bleaching semi-products, specification 20*10cm calculates dye liquor total amount according to the bath raio of 1:20, according still further to 5g/L
It is incremented by from 0-20g/L and weighs 5 anion-modified hyperbranched silicone softening agents, claims according still further to the dosage of 2% o.w.f of disperse yellow
Disperse dyes are taken to be added separately in 150mL dye model machine Dyeing pipe in order；
After disperse dye solutions at 40 DEG C are shaken up, with the acetum diluted adjust the dyestuff pH value in each Dyeing pipe to
6, it extracts, is put into dye liquor after then soaking fabric with water, Dyeing pipe is fitted into dye model machine, starting dye model machine, dye
Liquid is warming up to 130 DEG C of poststaining 30min, after cooling down, takes out fabric, is first washed with cold water, then carry out reduction cleaning, temperature is
85 DEG C, time 10min, bath raio 50:1, article is taken out in drying after cold water washes.
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