CN107338012A - Low-temperature environment-friendly imitates reactive adhesive and its preparation method and application - Google Patents
Low-temperature environment-friendly imitates reactive adhesive and its preparation method and application Download PDFInfo
- Publication number
- CN107338012A CN107338012A CN201710555465.7A CN201710555465A CN107338012A CN 107338012 A CN107338012 A CN 107338012A CN 201710555465 A CN201710555465 A CN 201710555465A CN 107338012 A CN107338012 A CN 107338012A
- Authority
- CN
- China
- Prior art keywords
- emulsion
- adhesive
- low
- imitates
- temperature environment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- 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
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- 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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
-
- 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
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of low-temperature environment-friendly to imitate reactive adhesive, by mass percentage including acrylic monomer, 35% 38%；Nanometer silicon emulsion, 1% 3%；Crosslinking agent, 0.5% 2%；Water soluble starter, 0.1% 0.5%；Anion emulsifier, 0.2% 0.5%；Nonionic emulsifier, 0.4% 1%；Deionized water, surplus.The invention also discloses the preparation method and application that a kind of low-temperature environment-friendly imitates reactive adhesive.
Description
Technical field
The present invention relates to fields such as weaving, chemistry, specially a kind of low-temperature environment-friendly imitates reactive adhesive and preparation method thereof
And application.
Background technology
Polyacrylate dispersion has excellent film forming, photostability and weatherability and good resistance to acid/base because of it
Property, water resistance, scratch resistance and caking property and be widely used in various industries, be mainly coating and coating print in field of textiles
The application of flower etc..
Textile printing and dyeing industry is constantly changed under environmentally friendly and economic overall situation, the keen competition in face of market, and dye-works is
Existence, energy-saving and emission-reduction are imperative, the requirement also more and more higher that becomes more meticulous of dyeing and printing process.Pigment printing is as printing technology
One kind, its environmental protection, energy-conservation and technological operation are simply increasingly favored by dye-works.
The pigment printing product of market can not replace the production of reactive printing completely still based on mid and low-end products at present
Product.Because the main performance of pigment printing is provided by adhesive, the performance quality of adhesive, Printing decide
Performance.In order to improve the quality of product, imitative reactive coating printing adhesive is also constantly pushed out, but can really be met imitative
The adhesive product of active feel and fastness requirement is few.What is had is soft, but dry/fastness to wet rubbing is very poor；Have
It is soft, phenomena such as doing/fastness to wet rubbing is qualified, but sticky net, plug net occur；This is all adhesive existing defects
Reason causes, and this can have a strong impact on the operating efficiency of dye-works, or even unnecessary loss may be brought to dye-works.In addition,
Present pigment printing is all high-temperature shaping, has been short of in terms of energy consumption is saved.
Therefore, on the premise of the normal operating efficiency of dye-works is not influenceed, while meet imitative reactive coating stamp requirement, make
Can partly replace or all instead of reactive printing, such low temperature imitate reactive coating printing adhesive have it is wide should
Use prospect.
The content of the invention
The purpose of the present invention is：A kind of low-temperature environment-friendly is provided and imitates reactive adhesive, makes it possible to part replacement or whole
Instead of reactive printing, to solve at least one technical problem of the prior art.
Realizing the technical scheme of above-mentioned purpose is：A kind of low-temperature environment-friendly imitates reactive adhesive, by mass percentage including third
Alkene acrylic monomer, 35%-38%；Nanometer silicon emulsion, 1%-3%；Crosslinking agent, 0.5%-2%；Water soluble starter, 0.1%-0.5%；It is cloudy
Ionic emulsifying agent, 0.2%-0.5%；Nonionic emulsifier, 0.4%-1%；Deionized water, surplus.
In a preferred embodiment of the present invention, the acrylic ester monomer includes butyl acrylate, ethyl acrylate, third
At least one of the different monooctyl ester of olefin(e) acid, acrylic acid, itaconic acid, acrylonitrile or methyl methacrylate.
In a preferred embodiment of the present invention, the nanometer silicon emulsion be by meteorological white carbon by coating emulsion dispersion and
Into water-dispersible emulsion.
In a preferred embodiment of the present invention, the crosslinking agent includes methacrylic acid acetoacetate epoxide ethyl ester, methyl
At least one of hydroxy-ethyl acrylate or DAAM.
In a preferred embodiment of the present invention, the water soluble starter includes one in potassium peroxydisulfate or sodium peroxydisulfate
Kind.
In a preferred embodiment of the present invention, the anion emulsifier includes double alkyl sulfosuccinics of the base containing double bond
At least one of ester salt, lauryl sodium sulfate；The nonionic emulsifier includes AEO, isomery C13
At least one of AEO.
The second object of the present invention is：The preparation method that a kind of described low-temperature environment-friendly imitates reactive adhesive is provided.
Realizing the technical scheme of the second purpose is：A kind of described low-temperature environment-friendly imitates the preparation method of reactive adhesive, bag
Include following steps：Step S1）Obtain raw material：Acrylic monomer, nanometer silicon emulsion, crosslinking agent, water are weighed by mass percentage
Soluble initiator, nonionic emulsifier, deionized water；Step S2）Prepare pre-emulsion；The step S2）Comprise the following steps, walk
Rapid S21）By step S1）In 97% or more amount of acrylic ester monomer, the full dose of crosslinking agent, anion emulsifier
Half, the full dose of nonionic emulsifier, 1/3rd of water soluble starter, 1/3rd of deionized water are added to instead
Answer in bottle；Step S22）At normal temperatures, stirred by mixer with 1500rpm-2000rpm rotating speed, mixing time is
20min-40min；Step S23）Emulsified by homogenizer, emulsification times are 20 min-40min, and the pre-emulsion is made；Step
S3）Prepare seed backing material；The step S3）Comprise the following steps, step S31）Weigh step S2）The four of middle pre-emulsion/
One adds in four-hole boiling flask；Step S32）By step S1）In acrylic ester monomer surplus, three points of water soluble starter
One of and remaining anion emulsifier, deionized water add into the four-hole boiling flask；Step S33）In described four mouthfuls burnings
Thermometer, condenser pipe, nitrogen tube are configured on bottle, and the solution in the four-hole boiling flask is slowly stirred by mixer；Step S4）
Produce adhesive；The step S4）Comprise the following steps, step S41）Nitrogen protection is passed through into the four-hole boiling flask, simultaneously
Heating water bath is warming up to 80 DEG C -83 DEG C, the uniform speed slow stirring of control mixer；Step S42）80 DEG C -83 DEG C are maintained the temperature at, drop
Add remaining pre-emulsion, until dripping off, time for adding 3h-3.5h；Step S43）By step S1）In remaining water soluble starter
The aqueous solution is configured to deionized water, the aqueous solution is added drop-wise in the four-hole boiling flask, and is warming up to 86 DEG C -88 DEG C, and is protected
Temperature, soaking time 2h-3h；；Step S44）20 DEG C -50 DEG C are cooled to, regulation pH value to 7-8；Step S45）To described four mouthfuls
Step S1 is added in flask）In the nanometer silicon emulsion full dose, persistently stir 20min-30min, be made adhesive mixing
Liquid；Step S46）With filter screen filtration, the sticky adhesive agent emulsion of obtained blue and white.
In a preferred embodiment of the present invention, the step S44）Including being passed through ammonia into the four-hole boiling flask, regulation
PH value is to 7-8.
In a preferred embodiment of the present invention, described adhesive emulsion accounts for the 38%- of described adhesive mixed liquor gross mass
40%.
The third object of the present invention is：The application that a kind of low-temperature environment-friendly imitates reactive adhesive is provided, applied to woven face
The imitative reactive coating stamp of material arranges, and stamp arranges：Under conditions of low-temperature curing, formed using the adhesive in fabric face
One layer water-fast, scrubbing resistance, the film of good toughness, and the temperature that wherein low temperature bakees is maintained at 115 DEG C -125 DEG C.
It is an advantage of the invention that：The low-temperature environment-friendly of the present invention imitates reactive adhesive and its preparation method and application, the feature of environmental protection
Can be good, reach international standard, particularly the requirement of the developed country such as Europe, the U.S., Japan；At adhesive by the present invention
The weaving face fabric managed, its is soft, and stamp is dry/and fastness to wet rubbing is good；The adhesive of the present invention is in use, can be with low temperature
（115℃-125℃）Film forming is crosslinked, amount of activated Printing can be replaced, and save energy consumption.
Embodiment
Embodiment, a kind of low-temperature environment-friendly imitates reactive adhesive, by mass percentage including acrylic monomer, 35%-
38%；Nanometer silicon emulsion, 1%-3%；Crosslinking agent, 0.5%-2%；Water soluble starter, 0.1%-0.5%；Anion emulsifier,
0.2%-0.5%；Nonionic emulsifier, 0.4%-1%；Deionized water, surplus.
In the present embodiment, the acrylic ester monomer include butyl acrylate, ethyl acrylate, Isooctyl acrylate monomer,
At least one of acrylic acid, itaconic acid, acrylonitrile or methyl methacrylate.The nanometer silicon emulsion is by meteorological white carbon
The water-dispersible emulsion formed by coating emulsion dispersion.The crosslinking agent include methacrylic acid acetoacetate epoxide ethyl ester,
At least one of hydroxyethyl methacrylate or DAAM.The water soluble starter includes potassium peroxydisulfate or mistake
One kind in sodium sulphate.The anion emulsifier includes double alkyl sulfosuccinates salt, the dodecyl sulphur of the base containing double bond
At least one of sour sodium；The nonionic emulsifier includes AEO, isomery C13 AEOs
At least one of.
Embodiment of the method 1, specifically comprises the following steps.
Step S1）Obtain raw material：Raw material is weighed by mass percentage：Acrylic monomer（Butyl acrylate 112g, propylene
The different monooctyl ester 20g of acid, methyl methacrylate 35g, acrylic acid 10g）177g；Nanometer silicon emulsion 10g；Crosslinking agent（Methacrylic acid
Acetoacetate epoxide ethyl ester 6g）6g；Water soluble starter（Sodium peroxydisulfate 1.2g）1.2g；Anion emulsifier（Alkyl sulfobetaines amber
Amber acid esters salt 0.5g, the base containing double bond double alkyl sulfosuccinates salt 0.5g）1g；Nonionic emulsifier（Fatty alcohol polyoxy second
Alkene ether 1.8g）1.8g；Deionized water 270g.
Step S2）Prepare pre-emulsion, the step S2）Comprise the following steps.
Step S21）By step S1）In acrylic ester monomer full dose（Butyl acrylate 112g, Isooctyl acrylate monomer
20g, methyl methacrylate 35g, acrylic acid 10g）, crosslinking agent full dose（Methacrylic acid acetoacetate epoxide ethyl ester 6g）、
Anion emulsifier（Alkyl sulfosuccinates salt 0.5g）, nonionic emulsifier（AEO 1.8g）, it is water-soluble
Property initiator（Sodium peroxydisulfate 0.4g）, deionized water（87g）It is added in reaction bulb.
Step S22）At normal temperatures, stirred by mixer with 1500rpm-2000rpm rotating speed, mixing time is
20min-40min。
Step S23）Emulsified by homogenizer, emulsification times 20min-40min, the pre-emulsion is made.
Step S3）Prepare seed backing material；The step S2）Comprise the following steps.
Step S31）Weigh step S2）The a quarter of middle pre-emulsion is added in four-hole boiling flask.
Step S32）By step S1）In water soluble starter（Sodium peroxydisulfate 0.4g）And remaining anion emulsifier
（Double alkyl sulfosuccinates salt 0.5g of the base containing double bond）, deionized water 173g added into the four-hole boiling flask.
Step S33）Thermometer, condenser pipe, nitrogen tube are configured on the four-hole boiling flask, and is slowly stirred by mixer
Solution in the four-hole boiling flask.
Step S4）Adhesive is made；The step S4）Comprise the following steps.
Step S41）Nitrogen protection is passed through into the four-hole boiling flask, while heating water bath is warming up to 80 DEG C -83 DEG C, control
Mixer uniform speed slow stirs.
Step S42）80 DEG C -83 DEG C are maintained the temperature at, remaining pre-emulsion is added dropwise, until dripping off, time for adding 3h-
3.5h。
Step S43）By step S1）In remaining water soluble starter（Sodium peroxydisulfate 0.4g）Configured with deionized water 10g
It is added drop-wise into the aqueous solution, and by the aqueous solution in the four-hole boiling flask, is warming up to 86 DEG C -88 DEG C, and be incubated, soaking time is
2h。
Step S44）Be cooled to less than 50 DEG C, be passed through into the four-hole boiling flask ammonia or add ammoniacal liquor, regulation pH value to
7-8。
Step S45）Step S1 is added into the four-hole boiling flask）In the nanometer silicon emulsion 10g, lasting stirring
30min, adhesive mixed liquor is made.
Step S46）After stirring terminates, the strainer filtering of used 120 mesh, the sticky adhesive agent emulsion of obtained blue and white.
Wherein described adhesive emulsion accounts for the 38%-40% of described adhesive mixed liquor gross mass.
Embodiment of the method 2
Specifically comprise the following steps.
Step S1）Obtain raw material：Raw material is weighed by mass percentage：Acrylic monomer（Butyl acrylate 112g, propylene
Acid different monooctyl ester 18g, methyl methacrylate 37g, acrylic acid 10g）177g；Nanometer silicon emulsion 10g；Crosslinking agent（Methacrylic acid
Hydroxyl ethyl ester 6g）6g；Water soluble starter（Sodium peroxydisulfate 1.2g）1.2g；Anion emulsifier（Lauryl sodium sulfate 1g）1g；
Nonionic emulsifier（AEO 1.8g）1.8g；Deionized water 270g.
Step S2）Prepare pre-emulsion, the step S2）Comprise the following steps.
Step S21）By step S1）In acrylic ester monomer full dose（Butyl acrylate 112g, Isooctyl acrylate monomer
18g, methyl methacrylate 37g, acrylic acid 10g）, crosslinking agent full dose（Hydroxyethyl methacrylate 6g）, it is anionic emulsifying
Agent（Lauryl sodium sulfate 0.5g）, nonionic emulsifier（AEO 1.8g）, water soluble starter（Persulfuric acid
Sodium 0.4g）, deionized water（87g）It is added in reaction bulb.
Step S22）At normal temperatures, stirred by mixer with 1500rpm-2000rpm rotating speed, mixing time is
20min-40min。
Step S23）Emulsified by homogenizer, emulsification times 20min-40min, the pre-emulsion is made.
Step S3）Prepare seed backing material；The step S2）Comprise the following steps.
Step S31）Weigh step S2）The a quarter of middle pre-emulsion is added in four-hole boiling flask.
Step S32）By step S1）In water soluble starter（Sodium peroxydisulfate 0.4g）And remaining anion emulsifier
（Lauryl sodium sulfate 0.5g）, deionized water 173g added into the four-hole boiling flask.
Step S33）Thermometer, condenser pipe, nitrogen tube are configured on the four-hole boiling flask, and is slowly stirred by mixer
Solution in the four-hole boiling flask.
Step S4）Prepare adhesive；The step S4）Comprise the following steps.
Step S41）Nitrogen protection is passed through into the four-hole boiling flask, while heating water bath is warming up to 80 DEG C -83 DEG C, control
Mixer uniform speed slow stirs.
Step S42）80 DEG C -83 DEG C are maintained the temperature at, remaining pre-emulsion is added dropwise, until dripping off, time for adding 3h-
3.5h。
Step S43）By step S1）In remaining water soluble starter（Sodium peroxydisulfate 0.4g）Configured with deionized water 10g
It is added drop-wise into the aqueous solution, and by the aqueous solution in the four-hole boiling flask, is warming up to 86 DEG C -88 DEG C, and be incubated, soaking time is
2h。
Step S44）Be cooled to less than 50 DEG C, be passed through into the four-hole boiling flask ammonia or add ammoniacal liquor, regulation pH value to
7-8。
Step S45）Step S1 is added into the four-hole boiling flask）In the nanometer silicon emulsion 10g, lasting stirring
30min, adhesive mixed liquor is made.
Step S46）After stirring terminates, the strainer filtering of used 120 mesh, the sticky adhesive agent emulsion of obtained blue and white.
Wherein described adhesive emulsion accounts for the 38%-40% of described adhesive mixed liquor gross mass.
Embodiment of the method 3
Specifically comprise the following steps.
Step S1）Obtain raw material：Raw material is weighed by mass percentage：Acrylic monomer（Butyl acrylate 110g, propylene
Acid different monooctyl ester 18g, methyl methacrylate 39g, acrylic acid 10g）177g；Nanometer silicon emulsion 10g；Crosslinking agent（Diacetone acrylamide
Acid amides 6g）6g；Water soluble starter（Sodium peroxydisulfate 1.2g）1.2g；Anion emulsifier（Lauryl sodium sulfate 1g）1g；It is non-
Ionic emulsifying agent（AEO 1.8g）1.8g；Deionized water 270g.
Step S2）Prepare pre-emulsion, the step S2）Comprise the following steps.
Step S21）By step S1）In acrylic ester monomer full dose（Butyl acrylate 110g, Isooctyl acrylate monomer
18g, methyl methacrylate 39g, acrylic acid 10g）, crosslinking agent full dose（DAAM 6g）, anion emulsifier
（Lauryl sodium sulfate 0.5g）, nonionic emulsifier（AEO 1.8g）, water soluble starter（Sodium peroxydisulfate
0.4g）, deionized water（87g）It is added in reaction bulb.
Step S22）At normal temperatures, stirred by mixer with 1500rpm-2000rpm rotating speed, mixing time is
20min-40min。
Step S23）Emulsified by homogenizer, emulsification times are 20 min-40min, and the pre-emulsion is made.
Step S3）Prepare seed backing material；The step S2）Comprise the following steps.
Step S31）Weigh step S2）The a quarter of middle pre-emulsion is added in four-hole boiling flask.
Step S32）By step S1）In water soluble starter（Sodium peroxydisulfate 0.4g）And remaining anion emulsifier
（Lauryl sodium sulfate 0.5g）, deionized water 173g added into the four-hole boiling flask.
Step S33）Thermometer, condenser pipe, nitrogen tube are configured on the four-hole boiling flask, and is slowly stirred by mixer
Solution in the four-hole boiling flask.
Step S4）Adhesive is made；The step S4）Comprise the following steps.
Step S41）Nitrogen protection is passed through into the four-hole boiling flask, while heating water bath is warming up to 80 DEG C -83 DEG C, control
Mixer uniform speed slow stirs.
Step S42）80 DEG C -83 DEG C are maintained the temperature at, remaining pre-emulsion is added dropwise, until dripping off, time for adding 3h-
3.5h。
Step S43）By step S1）In remaining water soluble starter（Sodium peroxydisulfate 0.4g）Configured with deionized water 10g
It is added drop-wise into the aqueous solution, and by the aqueous solution in the four-hole boiling flask, is warming up to 86 DEG C -88 DEG C, and be incubated, soaking time is
2h。
Step S44）Be cooled to less than 50 DEG C, be passed through into the four-hole boiling flask ammonia or add ammoniacal liquor, regulation pH value to
7-8。
Step S45）Step S1 is added into the four-hole boiling flask）In the nanometer silicon emulsion 10g, lasting stirring
30min, adhesive mixed liquor is made.
Step S46）After stirring terminates, the strainer filtering of used 120 mesh, the sticky adhesive agent emulsion of obtained blue and white.
Wherein described adhesive emulsion accounts for the 38%-40% of described adhesive mixed liquor gross mass.
Embodiment of the method 4
Specifically comprise the following steps.
Step S1）Obtain raw material：Raw material is weighed by mass percentage：Acrylic monomer（Butyl acrylate 107g, propylene
Acid different monooctyl ester 18g, methyl methacrylate 42g, acrylic acid 5g, itaconic acid 5g）177g；Nanometer silicon emulsion 10g；Crosslinking agent（It is double
Acetone acrylamide 6g）6g；Water soluble starter（Sodium peroxydisulfate 1.2g）1.2g；Anion emulsifier（Lauryl sodium sulfate
1g）1g；Nonionic emulsifier（Isomery C13 AEOs 1.8g）1.8g；Deionized water 270g.
Step S2）Prepare pre-emulsion, the step S2）Comprise the following steps.
Step S21）By step S1）In acrylic ester monomer（Butyl acrylate 107g, Isooctyl acrylate monomer 18g, first
Base methyl acrylate 42g, acrylic acid 5g）, crosslinking agent（DAAM 6g）, anion emulsifier（Dodecyl sulphate
Sodium 0.5g）, nonionic emulsifier（Isomery C13 AEOs 1.8g）, water soluble starter（Sodium peroxydisulfate 0.4g）、
Deionized water（87g）It is added in reaction bulb.
Step S22）At normal temperatures, stirred by mixer with 1500rpm-2000rpm rotating speed, mixing time is
20min-40min。
Step S23）Emulsified by homogenizer, emulsification times are 20 min-40min, and the pre-emulsion is made.
Step S3）Prepare seed backing material；The step S2）Comprise the following steps.
Step S31）Weigh step S2）The a quarter of middle pre-emulsion is added in four-hole boiling flask.
Step S32）By step S1）In acrylic ester monomer（Itaconic acid 5g）, water soluble starter（Sodium peroxydisulfate
0.4g）And remaining anion emulsifier（Lauryl sodium sulfate 0.5g）, deionized water 173g add to described four mouthfuls burning
In bottle.Wherein, itaconic acid is added in this step, is to increase internal stress and bridging property.
Step S33）Thermometer, condenser pipe, nitrogen tube are configured on the four-hole boiling flask, and is slowly stirred by mixer
Solution in the four-hole boiling flask.
Step S4）Adhesive is made；The step S4）Comprise the following steps.
Step S41）Nitrogen protection is passed through into the four-hole boiling flask, while heating water bath is warming up to 80 DEG C -83 DEG C, control
Mixer uniform speed slow stirs.
Step S42）80 DEG C -83 DEG C are maintained the temperature at, remaining pre-emulsion is added dropwise, until dripping off, time for adding 3h-
3.5h。
Step S43）By step S1）In remaining water soluble starter（Sodium peroxydisulfate 0.4g）Configured with deionized water 10g
It is added drop-wise into the aqueous solution, and by the aqueous solution in the four-hole boiling flask, is warming up to 86 DEG C -88 DEG C, and be incubated, soaking time is
2h。
Step S44）Be cooled to less than 50 DEG C, be passed through into the four-hole boiling flask ammonia or add ammoniacal liquor, regulation pH value to
7-8。
Step S45）Step S1 is added into the four-hole boiling flask）In the nanometer silicon emulsion 10g, lasting stirring
30min, adhesive mixed liquor is made.
Step S46）After stirring terminates, the strainer filtering of used 120 mesh, the sticky adhesive agent emulsion of obtained blue and white.
Wherein described adhesive emulsion accounts for the 38%-40% of described adhesive mixed liquor gross mass.
Application Example
The adhesive that above-described embodiment 1 to embodiment 4 is obtained is applied to cotton woven fabric pigment printing.
Using when, its technique includes：Stamp → drying（100℃×3min）→ bake（150 DEG C × 3min of high temperature, low temperature
120℃×3min）→ test（Dry/fastness to wet rubbing, feel, tinctorial yield and washing fastness）.
Mill base parameter is see table 1.
Table 1：Different adhesive mill base parameters.
| Market refers to sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Coating | 8% | 8% | 8% | 8% | 8% |
| Thickener | 1.625% | 1.431% | 1.425% | 1.435% | 1.475% |
| Adhesive | 20% | 20% | 20% | 20% | 20% |
| Water | 70.375% | 70.569% | 70.575% | 70.565% | 70.525% |
| Viscosity | 25000mPa·s | 25000mPa·s | 25000mPa·s | 25000mPa·s | 25000mPa·s |
The performance test results are see table 2 after different adhesive stamps.
Table 2：Performance comparison results of the 120 DEG C × 3min under the conditions of baking after different adhesive stamps.
| Dry fastness | Fastness to wet rubbing | Feel | Tinctorial yield | Washing fastness | |
| Market refers to sample | 2-2.5 level | 2 grades | It is soft | It is higher | Typically |
| Embodiment 1 | 3-3.5 level | 3 grades | It is soft | It is high | It is good |
| Embodiment 2 | 3-3.5 level | 3 grades | It is soft | It is high | It is good |
| Embodiment 3 | 3-3.5 level | 3 grades | It is soft | It is high | It is good |
| Embodiment 4 | 3.5-4 level | 3-3.5 level | It is soft | It is high | It is good |
It can be seen from above-mentioned table 2 under the conditions of 120 DEG C × 3min is baked, adhesive of the invention is relative in the market
It is existing refer to adhesive product, high level cadre/fastness to wet rubbing can be obtained after stamp, highly-flexible feel, high colouring quantity is good
Washing fastness.
Table 3：Performance comparison results of the 150 DEG C × 3min under the conditions of baking after different adhesive stamps.
| Dry fastness | Fastness to wet rubbing | Feel | Tinctorial yield | Washing fastness | |
| Market refers to sample | 3-3.5 level | 3 grades | It is soft | It is high | It is good |
| Embodiment 1 | 3.5-4 level | 3 grades | It is soft | It is high | It is good |
| Embodiment 2 | 3.5-4 level | 3 grades | It is soft | It is high | It is good |
| Embodiment 3 | 3.5-4 level | 3 grades | It is soft | It is high | It is good |
| Embodiment 4 | 4 grades | 3-3.5 level | It is soft | It is high | It is good |
As can be seen from Table 3, under the conditions of 150 DEG C × 3min is baked, the adhesive product of in the market does/fastness to wet rubbing
Lifting is obvious, can reach the performance of product under the conditions of 120 DEG C × 3min of invention adhesives low temperature is baked；But the present invention
Adhesive is under the conditions of 150 DEG C × 3min is baked, and dry/fastness to wet rubbing equally obtains certain raising, and performance is better than city
Field refers to sample；Illustrate the low-temperature adhesive product that the present invention designs, have better performance under the conditions of high temperature bakes.
In the present invention, selected by the collocation of raw material monomer, select specific crosslinking agent, and later stage to add one kind
Nanometer silicon emulsion obtains a kind of low temperature pigment printing binding agent, and it can be in fabric face under the conditions of 120 DEG C of low temperature bakes
One layer of water-fast, scrubbing resistance is formed, the film of good toughness, coating is so wrapped up and is attached to fabric face, because of the superiority of its own
Can, so as to assign the various bright patterns of fabric after stamp, and high scrubbing resistance fastness and washing fastness, highly-flexible can be obtained
The performance of feel.
Adhesive of the present invention compares existing various imitative reactive adhesives on the market, and its advantage is can be low
120 DEG C of temperature bakes condition and is issued to existing 150 DEG C of performances for baking pigment printing binding agent product on the market, ensure that coating
On the premise of the property indices of printing adhesive, energy-conserving and environment-protective, and the requirement of approximate active Printing can be obtained,
Or part replaces reactive printing product.
These are only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
All any modification, equivalent and improvement made within principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of low-temperature environment-friendly imitates reactive adhesive, it is characterised in that includes by mass percentage
Acrylic monomer, 35%-38%；
Nanometer silicon emulsion, 1%-3%；
Crosslinking agent, 0.5%-2%；
Water soluble starter, 0.1%-0.5%；
Anion emulsifier, 0.2%-0.5%；
Nonionic emulsifier, 0.4%-1%；
Deionized water, surplus.
2. low-temperature environment-friendly according to claim 1 imitates reactive adhesive, it is characterised in that the acrylic ester monomer bag
Include in butyl acrylate, ethyl acrylate, Isooctyl acrylate monomer, acrylic acid, itaconic acid, acrylonitrile or methyl methacrylate
It is at least one.
3. low-temperature environment-friendly according to claim 1 imitates reactive adhesive, it is characterised in that the nanometer silicon emulsion is by gas
The water-dispersible emulsion formed as white carbon by coating emulsion dispersion.
4. low-temperature environment-friendly according to claim 1 imitates reactive adhesive, it is characterised in that the crosslinking agent includes methyl-prop
At least one of olefin(e) acid acetoacetate epoxide ethyl ester, hydroxyethyl methacrylate or DAAM.
5. low-temperature environment-friendly according to claim 1 imitates reactive adhesive, it is characterised in that the water soluble starter includes
One kind in potassium peroxydisulfate or sodium peroxydisulfate.
6. low-temperature environment-friendly according to claim 1 imitates reactive adhesive, it is characterised in that the anion emulsifier includes
At least one of double alkyl sulfosuccinates salt of the base containing double bond, lauryl sodium sulfate；The nonionic emulsifier bag
Include at least one of AEO, isomery C13 AEOs.
7. a kind of low-temperature environment-friendly according to claim any one of 1-6 imitates the preparation method of reactive adhesive, its feature exists
In comprising the following steps：
Step S1）Obtain raw material：Acrylic monomer, nanometer silicon emulsion, crosslinking agent, water-soluble initiation are weighed by mass percentage
Agent, nonionic emulsifier, deionized water；
Step S2）Prepare pre-emulsion；The step S2）Comprise the following steps,
Step S21）By step S1）In 97% or more amount of acrylic ester monomer, the full dose of crosslinking agent, anion breast
The half of agent, the full dose of nonionic emulsifier, 1/3rd of water soluble starter, 1/3rd of deionized water add
Enter into reaction bulb；
Step S22）At normal temperatures, stirred by mixer with 1500rpm-2000rpm rotating speed, mixing time 20min-
40min；
Step S23）Emulsified by homogenizer, emulsification times are 20 min-40min, and the pre-emulsion is made；
Step S3）Prepare seed backing material；The step S3）Comprise the following steps,
Step S31）Weigh step S2）The a quarter of middle pre-emulsion is added in four-hole boiling flask；
Step S32）By step S1）In the surplus of acrylic ester monomer, 1/3rd of water soluble starter and it is cloudy from
The surplus of sub- emulsifying agent and 16/the 25 of deionized water additions are into the four-hole boiling flask；
Step S33）Thermometer, condenser pipe, nitrogen tube are configured on the four-hole boiling flask, and is slowly stirred by mixer described
Solution in four-hole boiling flask；
Step S4）Produce adhesive；The step S4）Comprise the following steps,
Step S41）Nitrogen protection is passed through into the four-hole boiling flask, while heating water bath is warming up to 80 DEG C -83 DEG C, control stirring
Machine uniform speed slow stirs；
Step S42）80 DEG C -83 DEG C are maintained the temperature at, remaining pre-emulsion is added dropwise, until dripping off, time for adding 3h-3.5h；
Step S43）By step S1）In remaining water soluble starter and deionized water be configured to the aqueous solution, by the water-soluble drop
It is added in the four-hole boiling flask, and is warming up to 86 DEG C -88 DEG C, and is incubated, soaking time 2h-3h；
Step S44）20 DEG C -50 DEG C are cooled to, regulation pH value to 7-8；
Step S45）Step S1 is added into the four-hole boiling flask）In the nanometer silicon emulsion full dose, lasting stirring
20min-30min, adhesive mixed liquor is made；
Step S46）With filter screen filtration, the sticky adhesive agent emulsion of obtained blue and white.
8. low-temperature environment-friendly according to claim 7 imitates the preparation method of reactive adhesive, it is characterised in that the step
S44）Including being passed through ammonia, regulation pH value to 7-8 into the four-hole boiling flask.
9. low-temperature environment-friendly according to claim 7 imitates the preparation method of reactive adhesive, it is characterised in that described adhesive
Emulsion accounts for the 38%-40% of described adhesive mixed liquor gross mass.
10. a kind of low-temperature environment-friendly according to claim any one of 1-6 imitates the application of reactive adhesive, applied to woven face
The imitative reactive coating stamp of material arranges；Stamp arranges：Under conditions of low-temperature curing, formed using the adhesive in fabric face
One layer water-fast, scrubbing resistance, the film of good toughness, and the temperature that wherein low temperature bakees is maintained at 115 DEG C -125 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710555465.7A CN107338012A (en) | 2017-07-10 | 2017-07-10 | Low-temperature environment-friendly imitates reactive adhesive and its preparation method and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710555465.7A CN107338012A (en) | 2017-07-10 | 2017-07-10 | Low-temperature environment-friendly imitates reactive adhesive and its preparation method and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107338012A true CN107338012A (en) | 2017-11-10 |
Family
ID=60219021
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710555465.7A Pending CN107338012A (en) | 2017-07-10 | 2017-07-10 | Low-temperature environment-friendly imitates reactive adhesive and its preparation method and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107338012A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591578A (en) * | 2019-09-27 | 2019-12-20 | 南京五人光学薄膜有限公司 | Water-soluble double-sided adhesive tape and double-sided adhesive tape cutting device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215356A (en) * | 2008-01-10 | 2008-07-09 | 江苏日出化工有限公司 | Nano silicon dioxide modified elastic acrylic ester copolymerization latex |
| CN104151486A (en) * | 2014-08-13 | 2014-11-19 | 陕西科技大学 | Method for preparing polyacrylic ester/nanoSiO2 coating printing adhesive by using Pickering emulsion polymerization method |
| CN105524225A (en) * | 2016-01-06 | 2016-04-27 | 上海保立佳新材料有限公司 | Core-shell type polyacrylate emulsion printing adhesive |
| CN105601801A (en) * | 2016-02-26 | 2016-05-25 | 厦门市德采化工科技有限公司 | Preparation process of acrylate resin emulsion having better abrasion-resistant performance and preparation process of corresponding compound printing mucilage |
-
2017
- 2017-07-10 CN CN201710555465.7A patent/CN107338012A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215356A (en) * | 2008-01-10 | 2008-07-09 | 江苏日出化工有限公司 | Nano silicon dioxide modified elastic acrylic ester copolymerization latex |
| CN104151486A (en) * | 2014-08-13 | 2014-11-19 | 陕西科技大学 | Method for preparing polyacrylic ester/nanoSiO2 coating printing adhesive by using Pickering emulsion polymerization method |
| CN105524225A (en) * | 2016-01-06 | 2016-04-27 | 上海保立佳新材料有限公司 | Core-shell type polyacrylate emulsion printing adhesive |
| CN105601801A (en) * | 2016-02-26 | 2016-05-25 | 厦门市德采化工科技有限公司 | Preparation process of acrylate resin emulsion having better abrasion-resistant performance and preparation process of corresponding compound printing mucilage |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591578A (en) * | 2019-09-27 | 2019-12-20 | 南京五人光学薄膜有限公司 | Water-soluble double-sided adhesive tape and double-sided adhesive tape cutting device |
| CN110591578B (en) * | 2019-09-27 | 2024-01-30 | 南京五人光学薄膜有限公司 | Water-soluble double-sided tape and double-sided tape cutting device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102060954B (en) | Acrylic emulsion as well as preparation method and application thereof | |
| CN103864976B (en) | The pre-emulsification semi-continuous seed emulsion polymerization technique of self-crosslinking styrene-acrylic emulsion for a kind of nonwoven | |
| CN102675558B (en) | Salt-resistive thickening agent as well as preparation method and application thereof | |
| CN102391411A (en) | Low-temperature self-crosslinking polyacrylate pigment printing binding agent and preparation method thereof | |
| CN105111363B (en) | A kind of function performed polymer and preparation method and application | |
| CN104910319B (en) | It is a kind of to delay polyacrylate dispersion of dye migration and preparation method thereof | |
| CN107964060A (en) | A kind of gradient type polyacrylate stamp lotion and preparation method thereof | |
| CN105696377A (en) | Efficient and rapid steaming printing technology adopting reactive dyes | |
| CN112574361B (en) | Preparation method of high-color-fastness water-based acrylate resin color paste, application and use method thereof | |
| CN103193922B (en) | A kind of water polyacrylic acid emulsion | |
| CN106758392A (en) | A kind of new dye stamp synthetic thickening agent and preparation method thereof, application | |
| CN107674148B (en) | Polyamide copolymer for printing nylon fabric | |
| CN101768880A (en) | Pearl powder printing paste composition, preparing method thereof and application thereof | |
| CN109293814A (en) | A kind of preparation method of the styrene-butadiene latex for papermaking paint | |
| CN106046242B (en) | A kind of aqueous environment protection flocking latex solution and its manufacturing method | |
| CN107338012A (en) | Low-temperature environment-friendly imitates reactive adhesive and its preparation method and application | |
| CN103233364B (en) | Self-cross-linking type waterborne polyacrylate powder-free base slurry for clothing fusible interlining | |
| CN103183774B (en) | A kind of seed emulsion preparation method | |
| CN108442141B (en) | Environment-friendly high-temperature foaming slurry special for printing and dyeing and preparation method thereof | |
| CN110791236B (en) | Water-based acrylate adhesive | |
| CN103183773B (en) | A kind of preparation method of water polyacrylic acid emulsion | |
| CN106749863B (en) | A kind of imitative reactive coating printing adhesive and preparation method thereof, application method | |
| CN114875695A (en) | Bio-based de-Guilin printing and discharging adhesive and preparation method and application thereof | |
| CN103183772B (en) | Method for preparing clothing adhesive lining from self-crosslinking water-borne polyacrylate powderless base mud | |
| CN103214617A (en) | Emulsion polymerization reaction method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171110 |