CN107964060A - A kind of gradient type polyacrylate stamp lotion and preparation method thereof - Google Patents
A kind of gradient type polyacrylate stamp lotion and preparation method thereof Download PDFInfo
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- CN107964060A CN107964060A CN201711137255.2A CN201711137255A CN107964060A CN 107964060 A CN107964060 A CN 107964060A CN 201711137255 A CN201711137255 A CN 201711137255A CN 107964060 A CN107964060 A CN 107964060A
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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
- C08F212/00—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 an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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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
- 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
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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
-
- 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
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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
- D06P1/5257—(Meth)acrylic acid
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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
- C08F220/16—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
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- Polymers & Plastics (AREA)
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polymerisation Methods In General (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of gradient type polyacrylate stamp lotion and preparation method thereof, which is prepared by the raw material of following mass parts：Hard monomer：30~105 parts；Soft monomer：50~120 parts；Function monomer：4~20 parts；Emulsifying agent：1~3 part；Initiator：0.5~3 part；PH buffer：0.2~1 part；Ammonium hydroxide：4~7；Water：130~180 parts.The gradient type polyacrylate stamp lotion of the present invention feeds emulsion polymerization technique by alternation and is prepared.The emulsion particle graded from soft to hard from inside to outside in the gradient type polyacrylate stamp lotion of the present invention, use it for the defects of pigment printing can be obviously improved acrylate " hot sticky cold crisp ", the performance indicators such as the feel of PRINTED FABRIC, colour fastness to rubbing, fastness to soaping are preferable, and APEO is free of in lotion, formaldehydeless release during use, environmentally protective, preparation process is simple, is suitable as high-grade environment-friendlyprinting printing adhesive.
Description
Technical field
The present invention relates to a kind of gradient type polyacrylate stamp lotion and preparation method thereof, belong to acrylic emulsion technology
Field.
Background technology
Pigment printing, also known as dry prints, are using high-molecular compound as adhesive, by certain processing, in fabric
It is upper to form a kind of transparent coloured film, the method for pigment fixation on the fabric.Pigment printing has that technique is simple, energy-saving
The advantages that water, suitable for various fibers and the stamp of blended fabric, such as drapery, home-textile, dress and personal adornment.
Acrylate adhesive be at present in pigment printing it is widely used one kind adhesive, since it contains
The functional groups such as carboxyl, ester group, thus it is strong to the adhesion of pigment and fiber, and also there is transparency height, good weatherability, price just
The advantages that suitable.However, acrylate adhesive has the problem of " hot sticky cold crisp ", low temperature becomes fragile, and high temperature becomes glutinous and loses by force, easily returns
It is glutinous, limit its application in high-grade fabric pigment printing.In addition, acrylate adhesive is used to be difficult to during pigment printing
The feel and fastness that have obtained at the same time, in order to obtain good fastness, it usually needs increase the dosage of crosslinking agent, but dosage of crosslinking agent
Increase feel can be made to be deteriorated again.Attempted by substantial amounts of, scientific research personnel has found：By core-shell emulsion synthetic technology, do not changing
Emulsion particle structure is adjusted on the premise of becoming emulsion monomer composition, can obtain and have excellent wearability and flexible stamp concurrently
Adhesive.However, the latex particle that nuclear-shell emulsion polymerization obtains is heterogeneous, tended to out after non-homogeneous structure film forming
The problems such as now film is opaque, seriously affects the quality of pigment printing.
The content of the invention
It is an object of the invention to provide a kind of gradient type polyacrylate stamp lotion and preparation method thereof.
The technical solution used in the present invention is：
A kind of gradient type polyacrylate stamp lotion, is prepared by the raw material of following mass parts：
Hard monomer：30~105 parts；
Soft monomer：50~120 parts；
Function monomer：4~20 parts；
Emulsifying agent：1~3 part；
Initiator：0.5~3 part；
PH buffer：0.2~1 part；
Ammonium hydroxide：4~7；
Water：130~180 parts.
The hard monomer is methyl methacrylate, methyl acrylate, vinylacetate, ethyl methacrylate, first
At least one of ester tert-butyl acrylate, acrylonitrile, styrene.
The soft monomer is ethyl acrylate, n-butyl acrylate, isobutyl acrylate, in Isooctyl acrylate monomer extremely
Few one kind.
The function monomer is acrylic acid, methacrylic acid, hydroxy-ethyl acrylate, hydroxyethyl methacrylate, propylene
Sour hydroxypropyl acrylate, hydroxy propyl methacrylate, glycidyl acrylate, glycidyl methacrylate, acrylamide, three hydroxyls
Trimethacrylate, tetraethylene-glycol dimethylacrylate, ethylene glycol dimethacrylate, Ji Wusi
At least one of alcohol triallyl ether.
The initiator is at least one of ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate.
The pH buffer is sodium acid carbonate.
The preparation method of above-mentioned gradient type polyacrylate stamp lotion comprises the following steps：
1) 0.5~3 part of initiator is dissolved in 30~40 parts of water, obtains initiator solution；
2) 0.5~1 part of emulsifying agent and 40~50 parts of water are uniformly mixed, add 4~30 parts of hard monomers, 33~100 parts
Soft monomer and 3~15 parts of function monomers, are uniformly mixed, obtain pre-emulsification monomer A；
3) 0.5~2 part of emulsifying agent and 30~40 parts of water are uniformly mixed, add 40~90 parts of hard monomers, 8~40 parts it is soft
Monomer and 5~15 parts of function monomers, are uniformly mixed, obtain pre-emulsification monomer B；
4) 0.2~1 part of emulsifying agent, 20~50 parts of water and 0.5~1 part of pH buffer are uniformly mixed, are warming up to 78~82
DEG C, 12~17 parts of pre-emulsification monomer A and 5~10 parts of initiator solutions are added, fully reaction, obtain seed emulsion；
5) seed emulsion is added into reactor, it is 80~90 DEG C to control temperature of reaction system, and it is molten that remaining initiator is added dropwise
Liquid, and pre-emulsification monomer B is added drop-wise in remaining pre-emulsification monomer A, while it is blended with the pre-emulsification list of pre-emulsification monomer B
Body A is added dropwise into reactor, then 0.5~1.5h of isothermal reaction, is cooled down after reaction, is added ammonium hydroxide and is adjusted pH value to 7~9, obtains
To gradient type polyacrylate stamp lotion.
The drop rate of initiator solution is 0.1~0.2 part/min in step 5), and pre-emulsification monomer B is added drop-wise to pre-emulsification
Drop rate in monomer A is 0.6~0.7 part/min, and the drop rate for being mixed with the pre-emulsification monomer A of pre-emulsification monomer B is
1.2~1.4 parts/min.
The beneficial effects of the invention are as follows：
1) present invention using " alternation charging " emulsion polymerization technique progress particle design, make in addition reaction system it is hard/
Soft monomer ratio is constantly incremental, so as to obtain the emulsion particle with gradient-structure, the emulsion particle ladder from soft to hard from inside to outside
Degree change, on the premise of transparency is ensured, efficiently solves the contradiction between polyacrylate stamp lotion feel and fastness,
The fastness and feel that PRINTED FABRIC has been provided simultaneously with；
2) the gradient type polyacrylate stamp lotion that the present invention is prepared is free of APEO, formaldehydeless during use to release
Put, it is environmentally protective；
3) preparation process of the invention is simple, workable, can be produced using general emulsion polymerization equipment, equipment
Invest small, be convenient for large-scale industrial production.
Brief description of the drawings
Fig. 1 is the structure diagram of the reactor in the present invention.
Embodiment
A kind of gradient type polyacrylate stamp lotion, is prepared by the raw material of following mass parts：
Hard monomer：30~105 parts；
Soft monomer：50~120 parts；
Function monomer：4~20 parts；
Emulsifying agent：1~3 part；
Initiator：0.5~3 part；
PH buffer：0.2~1 part；
Ammonium hydroxide：4~7；
Water：130~180 parts.
Preferably, the hard monomer is methyl methacrylate, methyl acrylate, vinylacetate, methacrylic acid
At least one of ethyl ester, methyl esters tert-butyl acrylate, acrylonitrile, styrene.
Preferably, the soft monomer be ethyl acrylate, n-butyl acrylate, isobutyl acrylate, acrylic acid it is different pungent
At least one of ester.
Preferably, the function monomer is acrylic acid, methacrylic acid, hydroxy-ethyl acrylate, hydroxyethyl methacrylate second
Ester, hydroxypropyl acrylate, hydroxy propyl methacrylate, glycidyl acrylate, glycidyl methacrylate, acryloyl
Amine, trimethylol-propane trimethacrylate, tetraethylene-glycol dimethylacrylate, ethylene glycol dimethacrylate
At least one of ester, pentaerythritol triallyl ether.
Preferably, the initiator is at least one of ammonium persulfate, potassium peroxydisulfate, sodium peroxydisulfate.
Preferably, the pH buffer is sodium acid carbonate.
The preparation method of above-mentioned gradient type polyacrylate stamp lotion comprises the following steps：
1) 0.5~3 part of initiator is dissolved in 30~40 parts of water, obtains initiator solution；
2) 0.5~1 part of emulsifying agent and 40~50 parts of water are uniformly mixed, add 4~30 parts of hard monomers, 33~100 parts
Soft monomer and 3~15 parts of function monomers, are uniformly mixed, obtain pre-emulsification monomer A；
3) 0.5~2 part of emulsifying agent and 30~40 parts of water are uniformly mixed, add 40~90 parts of hard monomers, 8~40 parts it is soft
Monomer and 5~15 parts of function monomers, are uniformly mixed, obtain pre-emulsification monomer B；
4) 0.2~1 part of emulsifying agent, 20~50 parts of water and 0.5~1 part of pH buffer are uniformly mixed, are warming up to 78~82
DEG C, 12~17 parts of pre-emulsification monomer A and 5~10 parts of initiator solutions are added, fully reaction, obtain seed emulsion；
5) seed emulsion is added into reactor, it is 80~90 DEG C to control temperature of reaction system, and it is molten that remaining initiator is added dropwise
Liquid, and pre-emulsification monomer B is added drop-wise in remaining pre-emulsification monomer A, while it is blended with the pre-emulsification list of pre-emulsification monomer B
Body A is added dropwise into reactor, then 0.5~1.5h of isothermal reaction, is cooled down after reaction, is added ammonium hydroxide and is adjusted pH value to 7~9, obtains
To gradient type polyacrylate stamp lotion.
Preferably, the time of reaction is 10~20min in step 4).
Preferably, the drop rate of initiator solution is 0.1~0.2 part/min in step 5), and pre-emulsification monomer B is added drop-wise to
Drop rate in pre-emulsification monomer A is 0.6~0.7 part/min, is mixed with the dropwise addition of the pre-emulsification monomer A of pre-emulsification monomer B
Speed is 1.2~1.4 parts/min.
The present invention is made further explanation and description with reference to specific embodiment.
Embodiment 1：
A kind of preparation method of gradient type polyacrylate stamp lotion, comprises the following steps：
1) 1.8 parts of initiators are dissolved in 40 parts of deionized waters, obtain initiator solution；
2) 1 part of emulsifying agent and 50 parts of deionized waters are mixed, 500rpm mechanical agitation 2min, add 20 parts of styrene,
50 parts of n-butyl acrylates, 20 parts of Isooctyl acrylate monomers, 5 parts of acrylamides, 3 parts of glycidyl methacrylate, 2.5 part third
Olefin(e) acid and 1 part of hydroxyethyl methacrylate, 800rpm mechanical agitation 15min, obtain pre-emulsification monomer A；
3) 1 part of emulsifying agent and 40 parts of deionized waters are mixed, 500rpm mechanical agitation 2min, add 45 parts of styrene, 2
Part methyl acrylate, 8 parts of n-butyl acrylates, 2 parts of Isooctyl acrylate monomers, 2 parts of acrylic acid, 2 parts of hydroxyethyl methacrylates and 2
Part trimethylol-propane trimethacrylate, 800rpm mechanical agitation 15min, obtain pre-emulsification monomer B；
4) 0.5 part of emulsifying agent, 35 parts of deionized waters and 0.5 part of sodium acid carbonate are uniformly mixed, are warming up to 80 DEG C, add
There is blue opalescence, obtain seed emulsion in 15 parts of pre-emulsification monomer A and 8 parts of initiator solutions, reaction 15min；
5) seed emulsion is added into reactor (as shown in Figure 1), controls temperature of reaction system as 85 DEG C, with peristaltic pump with
Remaining initiator solution is added dropwise in the drop rate of 0.15 part/min, and by pre-emulsification monomer B peristaltic pumps with 0.63 part/min
Drop rate be added drop-wise in remaining pre-emulsification monomer A, while be blended with the pre-emulsification monomer A of pre-emulsification monomer B with compacted
Dynamic pump is added dropwise into reactor with the drop rate of 1.3 parts/min, and isothermal reaction 0.8h, cools down after reaction, adds 4 parts of ammonium hydroxide
PH value is adjusted to 7~8,80 mesh filter screen filtering and dischargings, obtains gradient type polyacrylate stamp lotion.
Performance test：
Pure cotton fabric printing tests, stamp color are carried out using gradient type polyacrylate stamp lotion manufactured in the present embodiment
Slurry formula is following (mass percent)：Bright red mill base：2.5%；Gradient type polyacrylate stamp lotion (solid content 51%)：
20%；Thickener：4.5%；Water：73%.Using the table printing method of conventional manual plain net scraper, after 80 DEG C of preliminary drying 3min
130 DEG C bake 4min, then are tested, and the content of formaldehyde, fabric color fastness, feel test result after stamp are as shown in the table：
Table 1 is to the content of formaldehyde after pure cotton fabric stamp, fabric color fastness, feel test result
Embodiment 2：
A kind of preparation method of gradient type polyacrylate stamp lotion, comprises the following steps：
1) 1.5 parts of initiators are dissolved in 30 parts of deionized waters, obtain initiator solution；
2) 0.8 part of emulsifying agent and 40 parts of deionized waters are mixed, 500rpm mechanical agitation 2min, add 30 parts of methyl-props
E pioic acid methyl ester, 50 parts of n-butyl acrylates, 30 parts of ethyl acrylates, 5 parts of acrylamides, 3 parts of glycidyl methacrylate,
2 parts of acrylic acid and 1 part of hydroxyethyl methacrylate, 800rpm mechanical agitation 15min, obtain pre-emulsification monomer A；
3) 1.3 parts of emulsifying agents and 35 parts of deionized waters are mixed, 500rpm mechanical agitation 3min, add 50 parts of methyl-props
E pioic acid methyl ester, 15 parts of acrylonitrile, 10 parts of n-butyl acrylates, 16 parts of Isooctyl acrylate monomers, 5 parts of acrylic acid, 2 parts of methacrylic acids
Hydroxyl ethyl ester and 2 parts of trimethylol-propane trimethacrylates, 800rpm mechanical agitation 20min, obtain pre-emulsification monomer B；
4) 0.8 part of emulsifying agent, 25 parts of deionized waters and 1 part of sodium acid carbonate are uniformly mixed, are warming up to 80 DEG C, add 15
There is blue opalescence, obtain seed emulsion in part pre-emulsification monomer A and 8 parts of initiator solutions, reaction 15min；
5) seed emulsion is added into reactor (as shown in Figure 1), controls temperature of reaction system as 85 DEG C, with peristaltic pump with
Remaining initiator solution is added dropwise in the drop rate of 0.19 part/min, and by pre-emulsification monomer B peristaltic pumps with 0.7 part/min's
Drop rate is added drop-wise in remaining pre-emulsification monomer A, while the pre-emulsification monomer A for being blended with pre-emulsification monomer B is wriggled
Pump is added dropwise into reactor with the drop rate of 1.3 parts/min, and isothermal reaction 1.5h, cools down after reaction, adds 4 parts of ammonium hydroxide tune
PH value is saved to 7~8,80 mesh filter screen filtering and dischargings, obtains gradient type polyacrylate stamp lotion.
Performance test：
Pure cotton fabric printing tests, stamp color are carried out using gradient type polyacrylate stamp lotion manufactured in the present embodiment
Slurry formula is following (mass percent)：Bright red mill base：2.5%；Gradient type polyacrylate stamp lotion (solid content 51%)：
20%；Thickener：4.5%；Water：73%.Using the table printing method of conventional manual plain net scraper, after 80 DEG C of preliminary drying 3min
130 DEG C bake 4min, then are tested, and the content of formaldehyde, fabric color fastness, feel test result after stamp are as shown in the table：
Table 2 is to the content of formaldehyde after pure cotton fabric stamp, fabric color fastness, feel test result
Embodiment 3：
A kind of preparation method of gradient type polyacrylate stamp lotion, comprises the following steps：
1) 2.5 parts of initiators are dissolved in 35 parts of deionized waters, obtain initiator solution；
2) 0.7 part of emulsifying agent and 45 parts of deionized waters are mixed, 500rpm mechanical agitation 3min, add 15 parts of benzene second
Alkene, 10 parts of methyl methacrylates, 30 parts of isobutyl acrylates, 20 parts of Isooctyl acrylate monomers, 2.5 parts of acrylic acid and 1 part of methyl
Hydroxy-ethyl acrylate, 800rpm mechanical agitation 15min, obtain pre-emulsification monomer A；
3) 1 part of emulsifying agent and 30 parts of deionized waters are mixed, 500rpm mechanical agitation 2min, add 25 parts of styrene,
20 parts of methyl methacrylates, 10 parts of isobutyl acrylates, 2 parts of Isooctyl acrylate monomers, 2 parts of acrylic acid, 2 parts of hydroxyethyl methacrylates
Ethyl ester and 2 parts of trimethylol-propane trimethacrylates, 800rpm mechanical agitation 15min, obtain pre-emulsification monomer B；
4) 0.9 part of emulsifying agent, 45 parts of deionized waters and 0.7 part of sodium acid carbonate are uniformly mixed, are warming up to 80 DEG C, add
There is blue opalescence, obtain seed emulsion in 17 parts of pre-emulsification monomer A and 10 parts of initiator solutions, reaction 15min；
5) seed emulsion is added into reactor (as shown in Figure 1), controls temperature of reaction system as 85 DEG C, with peristaltic pump with
Remaining initiator solution is added dropwise in the drop rate of 0.16 part/min, and by pre-emulsification monomer B peristaltic pumps with 0.7 part/min's
Drop rate is added drop-wise in remaining pre-emulsification monomer A, while the pre-emulsification monomer A for being blended with pre-emulsification monomer B is wriggled
Pump is added dropwise into reactor with the drop rate of 1.2 parts/min, and isothermal reaction 1h, cools down after reaction, is added 3 parts of ammonium hydroxide and is adjusted
PH value obtains gradient type polyacrylate stamp lotion to 7~8,80 mesh filter screen filtering and dischargings.
Performance test：
Pure cotton fabric printing tests, stamp color are carried out using gradient type polyacrylate stamp lotion manufactured in the present embodiment
Slurry formula is following (mass percent)：Bright red mill base：2.5%；Gradient type polyacrylate stamp lotion (solid content 51%)：
20%；Thickener：4.5%；Water：73%.Using the table printing method of conventional manual plain net scraper, after 80 DEG C of preliminary drying 3min
130 DEG C bake 4min, then are tested, and the content of formaldehyde, fabric color fastness, feel test result after stamp are as shown in the table：
Table 3 is to the content of formaldehyde after pure cotton fabric stamp, fabric color fastness, feel test result
Comparative example：
A kind of preparation method of plain polypropylene acid esters stamp lotion, comprises the following steps：
1) 1.8 parts of initiators are dissolved in 40 parts of deionized waters, obtain initiator solution；
2) 1 part of emulsifying agent and 50 parts of deionized waters are mixed, 500rpm mechanical agitation 2min, add 40 parts of styrene,
30 parts of methyl methacrylates, 60 parts of butyl acrylates, 12 parts of Isooctyl acrylate monomers, 12 parts of methyl acrylates, 5 parts of acryloyls
Amine, 3 parts of glycidyl methacrylate, 4.5 parts of acrylic acid, 5 parts of acrylonitrile, 1 part of hydroxyethyl methacrylate and 2 part of three hydroxyl
Trimethacrylate, 800rpm mechanical agitation 15min, obtains pre-emulsification monomer；
3) 0.5 part of emulsifying agent, 35 parts of deionized waters and 0.5 part of sodium acid carbonate are uniformly mixed, are warming up to 80 DEG C, add
There is blue opalescence in 15 parts of pre-emulsification monomers and 8 parts of initiator solutions, reaction 15min, and it is 85 DEG C to control temperature of reaction system, and use is compacted
Remaining initiator solution is added dropwise in dynamic pump, while remaining pre-emulsification monomer, isothermal reaction 1h is added dropwise with peristaltic pump, and reaction terminates
After cool down, add 4 parts of ammonium hydroxide and adjust pH value to 7~8,80 mesh filter screen filtering and dischargings, obtain plain polypropylene acid esters stamp lotion.
Performance test：
The plain polypropylene acid esters stamp lotion prepared using this comparative example carries out pure cotton fabric printing tests, print paste
Formula is following (mass percent)：Bright red mill base：2.5%；Plain polypropylene acid esters stamp lotion (solid content 51%)：20%；
Thickener：4.5%；Water：73%.Using the table printing method of conventional manual plain net scraper, roasted for 130 DEG C after 80 DEG C of preliminary drying 3min
4min is dried, then is tested, the content of formaldehyde, fabric color fastness, feel test result after stamp are as shown in the table：
Table 4 is to the content of formaldehyde after pure cotton fabric stamp, fabric color fastness, feel test result
From table 1~4：The gradient type polyacrylate dispersion application that the present invention is prepared using alternation feeding process
In pigment printing, preferable fastness and feel can be obtained at the same time, and without APEO, formaldehydeless release is environmentally protective.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
- A kind of 1. gradient type polyacrylate stamp lotion, it is characterised in that：It is prepared by the raw material of following mass parts：Hard monomer：30~105 parts；Soft monomer：50~120 parts；Function monomer：4~20 parts；Emulsifying agent：1~3 part；Initiator：0.5~3 part；PH buffer：0.2~1 part；Ammonium hydroxide：4~7；Water：130~180 parts.
- 2. gradient type polyacrylate stamp lotion according to claim 1, it is characterised in that：The hard monomer is first Base methyl acrylate, methyl acrylate, vinylacetate, ethyl methacrylate, methyl esters tert-butyl acrylate, acrylonitrile, benzene At least one of ethene.
- 3. gradient type polyacrylate stamp lotion according to claim 1, it is characterised in that：The soft monomer is third At least one of olefin(e) acid ethyl ester, n-butyl acrylate, isobutyl acrylate, Isooctyl acrylate monomer.
- 4. gradient type polyacrylate stamp lotion according to claim 1, it is characterised in that：The function monomer is Acrylic acid, methacrylic acid, hydroxy-ethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, methacrylic acid hydroxypropyl Ester, glycidyl acrylate, glycidyl methacrylate, acrylamide, trimethylol-propane trimethacrylate, At least one in tetraethylene-glycol dimethylacrylate, ethylene glycol dimethacrylate, pentaerythritol triallyl ether Kind.
- 5. gradient type polyacrylate stamp lotion according to claim 1, it is characterised in that：The initiator was At least one of ammonium sulfate, potassium peroxydisulfate, sodium peroxydisulfate.
- 6. gradient type polyacrylate stamp lotion according to claim 1, it is characterised in that：The pH buffer is Sodium acid carbonate.
- 7. the preparation method of the gradient type polyacrylate stamp lotion in claim 1~6 described in any one, its feature exist In：Comprise the following steps：1) 0.5~3 part of initiator is dissolved in 30~40 parts of water, obtains initiator solution；2) 0.5~1 part of emulsifying agent and 40~50 parts of water are uniformly mixed, add 4~30 parts of hard monomers, 33~100 parts of soft lists Body and 3~15 parts of function monomers, are uniformly mixed, obtain pre-emulsification monomer A；3) 0.5~2 part of emulsifying agent and 30~40 parts of water are uniformly mixed, add 40~90 parts of hard monomers, 8~40 parts of soft monomers With 5~15 parts of function monomers, it is uniformly mixed, obtains pre-emulsification monomer B；4) 0.2~1 part of emulsifying agent, 20~50 parts of water and 0.5~1 part of pH buffer are uniformly mixed, are warming up to 78~82 DEG C, then 12~17 parts of pre-emulsification monomer A and 5~10 parts of initiator solutions, fully reaction are added, obtain seed emulsion；5) seed emulsion is added into reactor, it is 80~90 DEG C to control temperature of reaction system, and remaining initiator solution is added dropwise, and Pre-emulsification monomer B is added drop-wise in remaining pre-emulsification monomer A, while is blended with the pre-emulsification monomer A drops of pre-emulsification monomer B Reactor, then 0.5~1.5h of isothermal reaction are added, is cooled down after reaction, ammonium hydroxide is added and adjusts pH value to 7~9, obtain gradient Type polyacrylate stamp lotion.
- 8. preparation method according to claim 7, it is characterised in that：The drop rate of initiator solution is in step 5) 0.1~0.2 part/min, the drop rate that pre-emulsification monomer B is added drop-wise in pre-emulsification monomer A is 0.6~0.7 part/min, mixing The drop rate for having the pre-emulsification monomer A of pre-emulsification monomer B is 1.2~1.4 parts/min.
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| CN101696253A (en) * | 2009-10-27 | 2010-04-21 | 华南理工大学 | Acrylic ester polymer emulsion and preparation method thereof |
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| CN114539461A (en) * | 2022-02-21 | 2022-05-27 | 广东衡光新材料科技有限公司 | Acrylate emulsion with linear gradient structure, water-based industrial paint and preparation method thereof |
| CN114539461B (en) * | 2022-02-21 | 2023-11-10 | 广东衡光新材料科技有限公司 | Acrylate emulsion with linear gradient structure, water-based industrial paint and preparation method thereof |
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Application publication date: 20180427 |