CN107286287A - A kind of preparation method of pigment printing binding agent - Google Patents
A kind of preparation method of pigment printing binding agent Download PDFInfo
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- CN107286287A CN107286287A CN201710424704.5A CN201710424704A CN107286287A CN 107286287 A CN107286287 A CN 107286287A CN 201710424704 A CN201710424704 A CN 201710424704A CN 107286287 A CN107286287 A CN 107286287A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/06—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen
- C08F4/26—Metallic compounds other than hydrides and other than metallo-organic compounds; Boron halide or aluminium halide complexes with organic compounds containing oxygen of manganese, iron group metals or platinum group metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/44—Preparation of metal salts or ammonium salts
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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
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/525—Polymers of unsaturated carboxylic acids or functional derivatives thereof
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- Engineering & Computer Science (AREA)
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- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Coloring (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of preparation method of pigment printing binding agent, belong to printing and dyeing assistant preparing technical field.The present invention first by sodium lignin sulfonate and sodium hydroxide solution stirring preheating after with tetrabutyl titanate, the reaction discharging such as sodium pyrophosphate, collect out material and lyophilized ball milling after concussion is mixed with platinum nitrate, sieving particle and methyl acrylate are collected after sieving again, pre-emulsion is made in the stirring such as lecithin, again by part pre-emulsion and ammonium persulfate stirring reaction, remaining pre-emulsion is added dropwise again, and continuously add ammonium persulfate heating response, finally collect reactive material, pigment printing binding agent can be obtained, it is glutinous cold short that printing adhesive produced by the present invention effectively overcomes glued membrane heat, the not defect of stain resistant, assign the preferable feel of PRINTED FABRIC and higher resistance to dry, fastness to wet rubbing, and adhesive formaldehydeless release during preparation and use, to human body and environmentally friendly, have broad application prospects.
Description
Technical field
The invention discloses a kind of preparation method of pigment printing binding agent, belong to printing and dyeing assistant preparing technical field.
Background technology
Pigment printing is that coating is adhered into fiber surface by means of adhesive come the printing technology of pattern needed for obtaining, because
To have the advantages that technique is simple, chromatogram is complete, energy-saving, less pollution, increasingly paid attention to by dyeing, and
Used by increasing printing and dyeing mill.Water-based pigment printing/pigment dyeing technology is to meet the environmental protection of the strategy of sustainable development
Printing technology, is the developing direction of world's printing technology.Adhesive is the key component in pigment printing slurry, and its performance is straight
The stamp process of influence fabric is connect, fastness, feel and the style of PRINTED FABRIC is influenceed.
At present, Printing Industry adhesive is mostly water polyacrylic acid（PA）Class adhesive, because its have it is excellent into
Film, cementability, weatherability and guarantor's light colour retention, it has also become the class film forming being most widely used in weaving pigment printing material
Material.But, there is also not stain resistant, fastness to wet rubbing and the poor shortcoming of feel for this kind of printing adhesive, it is difficult to for height
Shelves Printing, and majority PA classes pigment printing binding agent all contains a certain amount of N hydroxymethyl acrylamide, is baking and is storing up
Meeting release formaldehyde during depositing, can be to health and environmental concerns, and which greatly limits printing adhesive
Application.Therefore, seek a kind of good environment-protection coating printing adhesive product of contaminated resistance to have important practical significance.
The content of the invention
Present invention mainly solves technical problem：For existing pigment printing binding agent not stain resistant, and baking and
During storage can release formaldehyde, to the defects of human body and environmental concerns, there is provided a kind of system of pigment printing binding agent
Preparation Method.
In order to solve technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of pigment printing binding agent, it is characterised in that specifically preparation process is：
（1）In mass ratio 1:4, it is that 15% sodium hydroxide solution is put into reactor to take sodium lignin sulfonate and mass fraction, is set
Temperature is 80~90 DEG C, stirring 10~15min of preheating, and tetrabutyl titanate is added into reactor, continues to stir 30~35min,
The gas in reactor is discharged using nitrogen, sodium pyrophosphate and VTES, heating are added into reactor
To 120~130 DEG C, 4~6h of stirring reaction is cooled to room temperature with 5 DEG C/min speed, is discharged, collect out material；
（2）In mass ratio 5:1~7:1, material will be gone out and be put into platinum nitrate in container, and container is placed in ultrasonic oscillation device
In, with 1.8~2.1MHz frequency oscillations, then the material in container is freeze-dried, collects freeze-drying thing；
（3）Freeze-drying thing is put into ball mill and carries out ball milling, ball-milled mixtures are collected, then ball-milled mixtures are crossed into 200 mesh
Sieve, collects sieving particle；
（4）Count by weight, take 90~95 parts of deionized waters, 60~65 parts of methyl acrylates, 30~34 parts of butyl acrylates,
15~20 parts of methyl methacrylates, 11~16 parts of sieving particles, 4~7 parts of lecithin and 3~6 parts of tetraethyl orthosilicates, are removed
Ionized water, methyl acrylate and lecithin are put into mixer and stirred, then addition butyl acrylate, metering system into mixer
Sour methyl esters, sieving particle and tetraethyl orthosilicate, stir 30~50min, obtain pre-emulsion；
（5）2/5ths of pre-emulsion volume is taken to be put into the four-hole boiling flask with agitator, thermometer and dropping funel, then
The ammonium persulfate of the quality such as tetraethyl orthosilicate is added into four-hole boiling flask, and four-hole boiling flask is moved in water-bath, setting temperature
Spend for 60~65 DEG C, stir 40~45min, reuse dropping funel and remaining pre-emulsion is added dropwise in four-hole boiling flask, be added dropwise
Speed is per second one drop；
（6）After emulsion is added dropwise to complete, the persulfuric acid of pre-emulsion quality 5~8% be added dropwise is added into four-hole boiling flask
Ammonium, is warming up to 78~82 DEG C, continues to stir 3h, then stands 2~3h, is cooled to room temperature, collects material in four-hole boiling flask, you can
Pigment printing binding agent.
The tetrabutyl titanate addition is the 15~20% of sodium lignin sulfonate quality.
The quality of the sodium pyrophosphate and VTES is equal, and is the 3 of sodium lignin sulfonate quality
~5%.
The temperature of the freeze-drying is -25~-15 DEG C, and vacuum is 10~15Pa.
The beneficial effects of the invention are as follows：
（1）The present invention is under alkaline environment, using sodium lignin sulfonate as surfactant, tetrabutyl titanate and the second of vinyl three
TMOS forms titanium hybrid silicon resinoid as raw material, while being complexed platinum ion using sodium pyrophosphate, makes titanium hybrid silicon class tree
Fat loads platinum ion, increases catalytic efficiency, improves stain resistance；
（2）The present invention is using methyl acrylate, butyl acrylate etc. as Material synthesis water polyacrylic acid, to sieve on particle
Platinum ion be catalyzed as catalyst, while with lecithin carry out surface active, by the use of ammonium persulfate as initiator, enter
Row synthesis, it is to avoid the generation of formaldehyde；
（3）Pigment printing binding agent produced by the present invention has excellent dry, fastness to wet rubbing and washing fastness, and the present invention is former
Expect environmental protection, the formaldehydeless release during preparing, baking and storing, to human body and environment non-hazardous；
（4）Pigment printing binding agent produced by the present invention is applied widely, it is adaptable to which roller, cylinder, plain net, hand printing etc. are more
Printing technology is planted, and obtained Printing is soft, flower-shape is clear-cut, lovely luster, meets people to textile printing
Higher and higher quality requirements.
Embodiment
In mass ratio 1:4, it is that 15% sodium hydroxide solution is put into reactor to take sodium lignin sulfonate and mass fraction, if
Constant temperature degree is 80~90 DEG C, with 120r/min stirring 10~15min of preheating, then the addition sodium lignin sulfonate quality into reactor
15~20% tetrabutyl titanate, is continued to stir 30~35min, is discharged the gas in reactor using nitrogen, then respectively to anti-
Answer the vinyl triethoxyl silicon that the quality such as the sodium pyrophosphate and sodium pyrophosphate of sodium lignin sulfonate quality 3~5% are added in kettle
Alkane, is warming up to 120~130 DEG C, with 200r/min 4~6h of stirring reaction, is cooled to room temperature with 5 DEG C/min speed, is discharged,
Collect out material, in mass ratio 5:1~7:1, material will be gone out and be put into platinum nitrate in container, and container is placed in ultrasonic oscillation
In device, with 1.8~2.1MHz, 40~50min of frequency oscillation, after ultrasonic vibration terminates, the material in container is put into vacuum cold
It is freeze-dried in lyophilizer, design temperature is -25~-15 DEG C, vacuum is 10~15Pa, collects freeze-drying thing,
And be put into ball mill, a diameter of 60mm of 6~9 times of lyophilized substance amount steel ball is added into ball mill, with 350r/
After 40~45min of min ball millings, ball-milled mixtures are crossed into 200 mesh sieves, sieving particle is collected, counts by weight, take 90~95 parts
Deionized water, 60~65 parts of methyl acrylates, 30~34 parts of butyl acrylates, 15~20 parts of methyl methacrylates, 11~16
Part sieving particle, 4~7 parts of lecithin and 3~6 parts of tetraethyl orthosilicates, remove ionized water, methyl acrylate and lecithin and are put into
In mixer, 10~15min, then addition butyl acrylate, methyl methacrylate, mistake into mixer are stirred with 400r/min
Particle and tetraethyl orthosilicate are sieved, 30~50min is stirred with 500r/min, pre-emulsion is obtained, then take the five of pre-emulsion volume
/ bis- are put into the four-hole boiling flask with agitator, thermometer and dropping funel, then add into four-hole boiling flask positive silicic acid four
The ammonium persulfate of the quality such as ethyl ester, and four-hole boiling flask is moved in water-bath, design temperature is 60~65 DEG C, is stirred with 120r/min
40~45min is mixed, dropping funel is reused and remaining pre-emulsion is added dropwise in four-hole boiling flask, drop rate is per second one drop,
Finally after emulsion is added dropwise to complete, the ammonium persulfate of pre-emulsion quality 5~8% be added dropwise is added into four-hole boiling flask, is risen
Temperature is incubated 2~3h to 78~82 DEG C, then is naturally cooling to room temperature, collects material in four-hole boiling flask, you can obtain pigment printing bonding
Agent.
Example 1
In mass ratio 1:4, it is that 15% sodium hydroxide solution is put into reactor to take sodium lignin sulfonate and mass fraction, setting temperature
Spend for 80 DEG C, 10min is preheated with 120r/min stirrings, then the metatitanic acid of sodium lignin sulfonate quality 15% is being added just into reactor
Butyl ester, is continued to stir 30min, is discharged the gas in reactor using nitrogen, then add sulfomethylated lignin into reactor respectively
The VTES of the quality such as the sodium pyrophosphate and sodium pyrophosphate of sour sodium quality 3%, is warming up to 120 DEG C, with 200r/
Min stirring reaction 4h, are cooled to room temperature with 5 DEG C/min speed, are discharged, collect out material, in mass ratio 5:1, it will discharge
Thing is put into container with platinum nitrate, and container is placed in ultrasonic oscillation device, with 1.8MHz frequency oscillation 40min, in ultrasound
After concussion terminates, the material in container is put into vacuum freeze drier and is freeze-dried, design temperature is -25 DEG C, very
Reciprocal of duty cycle is 10Pa, collects freeze-drying thing, and is put into ball mill, and the straight of 6 times of lyophilized substance amount is added into ball mill
Footpath is 60mm steel ball, after 350r/min ball millings 40min, and ball-milled mixtures are crossed into 200 mesh sieves, sieving particle is collected, by weight
Measure number meter, take 90 parts of deionized waters, 60 parts of methyl acrylates, 30 parts of butyl acrylates, 15 parts of methyl methacrylates, 11 parts
Sieve particle, 4 parts of lecithin and 3 parts of tetraethyl orthosilicates, removes ionized water, methyl acrylate and lecithin and is put into mixer
In, 10min is stirred with 400r/min, then add into mixer butyl acrylate, methyl methacrylate, sieving particle and just
Tetraethyl orthosilicate, stirs 30min with 500r/min, obtains pre-emulsion, then take 2/5ths of pre-emulsion volume to be put into and carry
In the four-hole boiling flask of agitator, thermometer and dropping funel, then add into four-hole boiling flask the mistake of the quality such as tetraethyl orthosilicate
Ammonium sulfate, and four-hole boiling flask is moved in water-bath, design temperature is 60 DEG C, stirs 40min with 120r/min, reuses dropping liquid
Remaining pre-emulsion is added dropwise in four-hole boiling flask by funnel, and drop rate is per second one drop, finally after emulsion is added dropwise to complete,
The ammonium persulfate of pre-emulsion quality 5% be added dropwise is added into four-hole boiling flask, 78 DEG C are warming up to, 2h, then Temperature fall is incubated
To room temperature, material in four-hole boiling flask is collected, you can obtain pigment printing binding agent.
Count by weight first, take 1 part of printing gum, 3 parts of dyestuffs, 10 parts of pigment printing binding agents produced by the present invention
With 35 parts of water, in the cylinder that is added sequentially to size mixing, and with 200r/min stirring mixing 10min, concentrator is obtained, then kiering is floated
Fabric after white is placed on workbench, and concentrator is printed on fabric using cylinder, treats after the completion of textile printing, will print
Fabric after spending bakes 2min at a temperature of 110 DEG C, then is cleaned fabric with 35 DEG C of water, finally takes out fabric and dries naturally i.e.
Can.After testing, fabric is carried out after stamp using pigment printing binding agent produced by the present invention, the dry, wet of fabric can be improved and rubbed
Rubbing fastness and fastness to washing, compared with using traditional coating printing adhesive, fabric is dry, fastness to wet rubbing improves 1 grade, resistance to
Wash fastness and improve 1 grade, while fabrics feel soft, lovely luster after stamp, and its equal nothing during preparation and use
Form aldehyde release, it is harmless to environment and human body.
Example 2
In mass ratio 1:4, it is that 15% sodium hydroxide solution is put into reactor to take sodium lignin sulfonate and mass fraction, setting temperature
Spend for 85 DEG C, 13min is preheated with 120r/min stirrings, then the metatitanic acid of sodium lignin sulfonate quality 18% is being added just into reactor
Butyl ester, is continued to stir 33min, is discharged the gas in reactor using nitrogen, then add sulfomethylated lignin into reactor respectively
The VTES of the quality such as the sodium pyrophosphate and sodium pyrophosphate of sour sodium quality 4%, is warming up to 125 DEG C, with 200r/
Min stirring reaction 5h, are cooled to room temperature with 5 DEG C/min speed, are discharged, collect out material, in mass ratio 6:1, it will discharge
Thing is put into container with platinum nitrate, and container is placed in ultrasonic oscillation device, with 2.0MHz frequency oscillation 45min, in ultrasound
After concussion terminates, the material in container is put into vacuum freeze drier and is freeze-dried, design temperature is -20 DEG C, very
Reciprocal of duty cycle is 13Pa, collects freeze-drying thing, and is put into ball mill, and the straight of 7 times of lyophilized substance amount is added into ball mill
Footpath is 60mm steel ball, after 350r/min ball millings 43min, and ball-milled mixtures are crossed into 200 mesh sieves, sieving particle is collected, by weight
Measure number meter, take 93 parts of deionized waters, 63 parts of methyl acrylates, 32 parts of butyl acrylates, 18 parts of methyl methacrylates, 14 parts
Sieve particle, 6 parts of lecithin and 5 parts of tetraethyl orthosilicates, removes ionized water, methyl acrylate and lecithin and is put into mixer
In, 13min is stirred with 400r/min, then add into mixer butyl acrylate, methyl methacrylate, sieving particle and just
Tetraethyl orthosilicate, stirs 40min with 500r/min, obtains pre-emulsion, then take 2/5ths of pre-emulsion volume to be put into and carry
In the four-hole boiling flask of agitator, thermometer and dropping funel, then add into four-hole boiling flask the mistake of the quality such as tetraethyl orthosilicate
Ammonium sulfate, and four-hole boiling flask is moved in water-bath, design temperature is 63 DEG C, stirs 43min with 120r/min, reuses dropping liquid
Remaining pre-emulsion is added dropwise in four-hole boiling flask by funnel, and drop rate is per second one drop, finally after emulsion is added dropwise to complete,
The ammonium persulfate of pre-emulsion quality 7% be added dropwise is added into four-hole boiling flask, 80 DEG C are warming up to, 2h, then Temperature fall is incubated
To room temperature, material in four-hole boiling flask is collected, you can obtain pigment printing binding agent.
Count by weight first, take 1 part of printing gum, 4 parts of dyestuffs, 14 parts of pigment printing binding agents produced by the present invention
With 42 parts of water, in the cylinder that is added sequentially to size mixing, and with 250r/min stirring mixing 13min, concentrator is obtained, then kiering is floated
Fabric after white is placed on workbench, and concentrator is printed on fabric using cylinder, treats after the completion of textile printing, will print
Fabric after spending bakes 3min at a temperature of 120 DEG C, then is cleaned fabric with 37 DEG C of water, finally takes out fabric and dries naturally i.e.
Can.After testing, fabric is carried out after stamp using pigment printing binding agent produced by the present invention, the dry, wet of fabric can be improved and rubbed
Rubbing fastness and fastness to washing, compared with using traditional coating printing adhesive, fabric is dry, fastness to wet rubbing improves 1 grade, resistance to
Wash fastness and improve 2 grades, while fabrics feel soft, lovely luster after stamp, and its equal nothing during preparation and use
Form aldehyde release, it is harmless to environment and human body.
Example 3
In mass ratio 1:4, it is that 15% sodium hydroxide solution is put into reactor to take sodium lignin sulfonate and mass fraction, setting temperature
Spend for 90 DEG C, 15min is preheated with 120r/min stirrings, then the metatitanic acid of sodium lignin sulfonate quality 20% is being added just into reactor
Butyl ester, is continued to stir 35min, is discharged the gas in reactor using nitrogen, then add sulfomethylated lignin into reactor respectively
The VTES of the quality such as the sodium pyrophosphate and sodium pyrophosphate of sour sodium quality 5%, is warming up to 130 DEG C, with 200r/
Min stirring reaction 6h, are cooled to room temperature with 5 DEG C/min speed, are discharged, collect out material, in mass ratio 7:1, it will discharge
Thing is put into container with platinum nitrate, and container is placed in ultrasonic oscillation device, with 2.1MHz frequency oscillation 50min, in ultrasound
After concussion terminates, the material in container is put into vacuum freeze drier and is freeze-dried, design temperature is -15 DEG C, very
Reciprocal of duty cycle is 15Pa, collects freeze-drying thing, and is put into ball mill, and the straight of 9 times of lyophilized substance amount is added into ball mill
Footpath is 60mm steel ball, after 350r/min ball millings 45min, and ball-milled mixtures are crossed into 200 mesh sieves, sieving particle is collected, by weight
Measure number meter, take 95 parts of deionized waters, 65 parts of methyl acrylates, 34 parts of butyl acrylates, 20 parts of methyl methacrylates, 16 parts
Sieve particle, 7 parts of lecithin and 6 parts of tetraethyl orthosilicates, removes ionized water, methyl acrylate and lecithin and is put into mixer
In, 15min is stirred with 400r/min, then add into mixer butyl acrylate, methyl methacrylate, sieving particle and just
Tetraethyl orthosilicate, stirs 50min with 500r/min, obtains pre-emulsion, then take 2/5ths of pre-emulsion volume to be put into and carry
In the four-hole boiling flask of agitator, thermometer and dropping funel, then add into four-hole boiling flask the mistake of the quality such as tetraethyl orthosilicate
Ammonium sulfate, and four-hole boiling flask is moved in water-bath, design temperature is 65 DEG C, stirs 45min with 120r/min, reuses dropping liquid
Remaining pre-emulsion is added dropwise in four-hole boiling flask by funnel, and drop rate is per second one drop, finally after emulsion is added dropwise to complete,
The ammonium persulfate of pre-emulsion quality 8% be added dropwise is added into four-hole boiling flask, 82 DEG C are warming up to, 3h, then Temperature fall is incubated
To room temperature, material in four-hole boiling flask is collected, you can obtain pigment printing binding agent.
Count by weight first, take 2 parts of printing gums, 5 parts of dyestuffs, 18 parts of pigment printing binding agents produced by the present invention
With 50 parts of water, in the cylinder that is added sequentially to size mixing, and with 300r/min stirring mixing 15min, concentrator is obtained, then kiering is floated
Fabric after white is placed on workbench, and concentrator is printed on fabric using cylinder, treats after the completion of textile printing, will print
Fabric after spending bakes 4min at a temperature of 130 DEG C, then is cleaned fabric with 40 DEG C of water, finally takes out fabric and dries naturally i.e.
Can.After testing, fabric is carried out after stamp using pigment printing binding agent produced by the present invention, the dry, wet of fabric can be improved and rubbed
Rubbing fastness and fastness to washing, compared with using traditional coating printing adhesive, fabric is dry, fastness to wet rubbing improves 2 grades, resistance to
Wash fastness and improve 2 grades, while fabrics feel soft, lovely luster after stamp, and its equal nothing during preparation and use
Form aldehyde release, it is harmless to environment and human body.
Claims (4)
1. a kind of preparation method of pigment printing binding agent, it is characterised in that specifically preparation process is：
（1）In mass ratio 1:4, it is that 15% sodium hydroxide solution is put into reactor to take sodium lignin sulfonate and mass fraction, is set
Temperature is 80~90 DEG C, stirring 10~15min of preheating, and tetrabutyl titanate is added into reactor, continues to stir 30~35min,
The gas in reactor is discharged using nitrogen, sodium pyrophosphate and VTES, heating are added into reactor
To 120~130 DEG C, 4~6h of stirring reaction is cooled to room temperature with 5 DEG C/min speed, is discharged, collect out material；
（2）In mass ratio 5:1~7:1, material will be gone out and be put into platinum nitrate in container, and container is placed in ultrasonic oscillation device
In, with 1.8~2.1MHz frequency oscillations, then the material in container is freeze-dried, collects freeze-drying thing；
（3）Freeze-drying thing is put into ball mill and carries out ball milling, ball-milled mixtures are collected, then ball-milled mixtures are crossed into 200 mesh
Sieve, collects sieving particle；
（4）Count by weight, take 90~95 parts of deionized waters, 60~65 parts of methyl acrylates, 30~34 parts of butyl acrylates,
15~20 parts of methyl methacrylates, 11~16 parts of sieving particles, 4~7 parts of lecithin and 3~6 parts of tetraethyl orthosilicates, are removed
Ionized water, methyl acrylate and lecithin are put into mixer and stirred, then addition butyl acrylate, metering system into mixer
Sour methyl esters, sieving particle and tetraethyl orthosilicate, stir 30~50min, obtain pre-emulsion；
（5）2/5ths of pre-emulsion volume is taken to be put into the four-hole boiling flask with agitator, thermometer and dropping funel, then
The ammonium persulfate of the quality such as tetraethyl orthosilicate is added into four-hole boiling flask, and four-hole boiling flask is moved in water-bath, setting temperature
Spend for 60~65 DEG C, stir 40~45min, reuse dropping funel and remaining pre-emulsion is added dropwise in four-hole boiling flask, be added dropwise
Speed is per second one drop；
（6）After emulsion is added dropwise to complete, the persulfuric acid of pre-emulsion quality 5~8% be added dropwise is added into four-hole boiling flask
Ammonium, is warming up to 78~82 DEG C, continues to stir 3h, then stands 2~3h, is cooled to room temperature, collects material in four-hole boiling flask, you can
Pigment printing binding agent.
2. a kind of preparation method of pigment printing binding agent according to claim 1, it is characterised in that：The positive fourth of metatitanic acid
Ester addition is the 15~20% of sodium lignin sulfonate quality.
3. a kind of preparation method of pigment printing binding agent according to claim 1, it is characterised in that：The sodium pyrophosphate
It is equal with the quality of VTES, and be the 3~5% of sodium lignin sulfonate quality.
4. a kind of preparation method of pigment printing binding agent according to claim 1, it is characterised in that：The freeze-drying
Temperature be -25~-15 DEG C, vacuum be 10~15Pa.
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| CN102344522A (en) * | 2011-06-25 | 2012-02-08 | 百利合化工（中山）有限公司 | Environment-friendly printing platen adhesive emulsion and preparation method thereof |
| CN102477119A (en) * | 2010-11-29 | 2012-05-30 | 武汉纺织大学 | Method for preparing environment-friendly pigment printing binder |
| CN102603963A (en) * | 2012-03-27 | 2012-07-25 | 陕西科技大学 | Preparation method of environmentally-friendly polyacrylic ester pigment printing adhesive |
| CN102757525A (en) * | 2012-07-25 | 2012-10-31 | 上海雅运纺织助剂有限公司 | Environmental-friendly pigment printing binding agent and preparation method thereof |
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2017
- 2017-06-07 CN CN201710424704.5A patent/CN107286287A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928367A (en) * | 2010-08-24 | 2010-12-29 | 华南理工大学 | Environmentally-friendly acrylic ester coating printing adhesive emulsion and preparation method |
| CN102477119A (en) * | 2010-11-29 | 2012-05-30 | 武汉纺织大学 | Method for preparing environment-friendly pigment printing binder |
| CN102344522A (en) * | 2011-06-25 | 2012-02-08 | 百利合化工（中山）有限公司 | Environment-friendly printing platen adhesive emulsion and preparation method thereof |
| CN102603963A (en) * | 2012-03-27 | 2012-07-25 | 陕西科技大学 | Preparation method of environmentally-friendly polyacrylic ester pigment printing adhesive |
| CN102757525A (en) * | 2012-07-25 | 2012-10-31 | 上海雅运纺织助剂有限公司 | Environmental-friendly pigment printing binding agent and preparation method thereof |
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Application publication date: 20171024 |