CN106832085A - A kind of high temperature resistant, high rigidity acrylate and vinyl acetate emulsion of color inhibition and preparation method thereof - Google Patents
A kind of high temperature resistant, high rigidity acrylate and vinyl acetate emulsion of color inhibition and preparation method thereof Download PDFInfo
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- CN106832085A CN106832085A CN201611267805.8A CN201611267805A CN106832085A CN 106832085 A CN106832085 A CN 106832085A CN 201611267805 A CN201611267805 A CN 201611267805A CN 106832085 A CN106832085 A CN 106832085A
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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
- C08F218/00—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 acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
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- C08F218/04—Vinyl esters
- C08F218/08—Vinyl acetate
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- 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
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- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
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- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C09J131/00—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 an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Adhesives based on derivatives of such polymers
- C09J131/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C09J131/04—Homopolymers or copolymers of vinyl acetate
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Abstract
The invention discloses a kind of high temperature resistant, the high rigidity acrylate and vinyl acetate emulsion of color inhibition, it includes water, butyl acrylate, vinylacetate, function monomer, N NMAs, emulsifying agent, persulfate.Said components are calculated as according to mass fraction：100 parts of water, 28 parts of butyl acrylate, 100 150 parts of vinylacetate, 15 parts of function monomer, 5 10 parts of N NMAs, 15 parts of emulsifying agent, 0.1 1 parts of persulfate.High temperature resistant of the invention, the high rigidity acrylate and vinyl acetate emulsion yellowing resistance of color inhibition and heat-resisting quantity are good, and with higher hardness.
Description
Technical field
The present invention relates to a kind of acrylic acid ester emulsion and preparation method thereof, specifically a kind of high temperature resistant, the height of color inhibition
Hardness acrylate and vinyl acetate emulsion and preparation method thereof.
Background technology
Gum sprayed cotton is that its principle is that adhesive is sprayed at into fluffy fibrage at present using quite varied non-weaving cloth
Two sides, because having certain pressure in spray, and suction during binding fiber layer lower vacuum imbibition, so in fibrage
Inside can also penetrate into adhesive, and the fibrage after spray adhesive by drying, solidification, is glued interfibrous interface point again
Connect, and the fiber not being bonded to each other, still there is sizable free degree.Because it has fluffy, compression resilience is high, resistance to dry, wet
Washing, and light weight and the performance such as warming, so turned into fabricating cotton clothes, space suit or cotton-wadded quilt, sleeping bag etc. in recent years
The important materials of bedding.In the production of gum sprayed cotton, because Vinyl Acetate Monomer is cheap, and can synthetic glass
Temperature acrylate and vinyl acetate emulsion higher, while it can provide bonding effect for glue spraying cotton fiber, prevents fibre shedding, and strengthen gum sprayed cotton
Gas permeability and improve resilience, thus acrylate and vinyl acetate emulsion gum sprayed cotton production in usage amount it is very huge.
However, acrylate and vinyl acetate emulsion itself has great technological deficiency.Due to all being needed in gum sprayed cotton nonwoven production process
Will be by 150 DEG C of high temperature drying and shapings, and acrylate and vinyl acetate emulsion resistance to elevated temperatures is excessively poor, and white fiber can be caused to occur becoming after drying
Yellow situation, so as to have a strong impact on the stability of fiber color.The easy xanthochromia reason of acrylate and vinyl acetate emulsion high temperature has two：
First, Vinyl Acetate Monomer is water-soluble larger in water, easily there is hydrolysis generation acetic acid after being dissolved in water.Acetic acid
In the presence of that can make, reaction conversion ratio is relatively low, causes emulsion monomer remnants quantitative changes big, and monomer itself is because containing double bond, in hot conditions
Under can be oxidized rapidly, so as to cause fiber xanthochromia.In addition, acetic acid is remained in the middle of emulsion in itself, similarly can be by under high temperature
Oxidation, and cause fiber xanthochromia.
Second, the carbonyl on acrylate and vinyl acetate emulsion macromolecular chain does not have other groups to protect, it is oxidized easily under hot conditions, is made
There is xanthochromia in fiber.Further, since carbonyl polarity is larger, the vapor in its easy absorption air makes product soften, so that greatly
Width reduce glue spraying cotton nonwoven fabrics into type hardness tester.
Therefore, a kind of color inhibition and high temperature resistant and the gum sprayed cotton emulsion with certain degree of hardness are researched and developed, is current acrylic acid
One technical barrier of ester emulsion manufacture.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of yellowing resistance and heat-resisting quantity are good, and have
There is the acrylate and vinyl acetate emulsion of higher hardness.
Another goal of the invention of the invention is to provide the method for preparing above-mentioned acrylate and vinyl acetate emulsion.
What goal of the invention of the invention was realized in：The high rigidity acrylate and vinyl acetate emulsion of a kind of high temperature resistant, color inhibition, its feature
It is：The high temperature resistant, color inhibition high rigidity acrylate and vinyl acetate emulsion include water, butyl acrylate, vinylacetate, function monomer,
N hydroxymethyl acrylamide, emulsifying agent, persulfate.Said components are calculated as according to mass fraction：100 parts of water, acrylic acid fourth
Ester 2-8 parts, vinylacetate 100-150 parts, function monomer 1-5 parts, N hydroxymethyl acrylamide 5-10 parts, emulsifying agent 1-5 parts,
Persulfate 0.1-1 parts.
The function monomer is for the one kind in hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid, itaconic acid or with any
Ratio mixes.
The emulsifying agent is for the one kind in AEO, phosphoric acid half ester ethoxylation disodium mixture or to appoint
Meaning ratio mixes.
The persulfate mixes for the one kind in sodium peroxydisulfate, ammonium persulfate, potassium peroxydisulfate or with arbitrary proportion.
The N hydroxymethyl acrylamide is 40-50% effective active composition liquid.
The high temperature resistant, the preparation method of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are comprised the following steps：
a）Raw material for standby is weighed according to said ratio；
b）30-40 parts of water, emulsifying agent, butyl acrylate, vinylacetate, function are added under normal temperature and pressure state in emulsion tank
Monomer and N hydroxymethyl acrylamide are simultaneously stirred well to uniform；
c）Excess water is added in a kettle., and temperature of reaction kettle is promoted to 65-70 DEG C, add the b step gained of 5-15% mixed
Compound, reacts 30-40 minutes；
d）Remaining b step gained mixture and persulfate is added dropwise toward step c gained mixture, reaction temperature is maintained at
75-80 DEG C and continue stirring, reaction time 3-5 hours；
e）80-85 DEG C is warming up to after Step d is added dropwise to complete, and is incubated 1-2 hours；
f）Obtain adding reductant-oxidant in mixture toward step e, be cooled to 70-75 DEG C, and be incubated 10-20 minutes；
g）Reductant-oxidant is added again toward mixture obtained in f steps, is cooled to 60-70 DEG C, and be incubated 10-20 minutes；
h）Mixture obtained in g steps is cooled to 40-50 DEG C, acrylic acid ester emulsion is obtained final product after filtering.
It is of the invention compared with traditional wall primer emulsion, with advantages below：
1st, in the high rigidity acrylate and vinyl acetate emulsion of high temperature resistant of the invention, color inhibition, long chain type acrylic acid reaction system is employed, and add
The N hydroxymethyl acrylamide extremely strong with reaction system compatibility is entered.First, the chemical bond energy of long chain type reaction system is higher,
And around double bond there is more protectiveness group to surround, oxidation is not susceptible in the high temperature drying and shaping operation of gum sprayed cotton anti-
Should, and strand can be avoided the situation of pyrolytic occur, so as to there is the phenomenon for turning yellow in white fiber after drying is greatly decreased.
Secondly, N hydroxymethyl acrylamide can disengage formaldehyde small molecule under the high temperature conditions, and it is anti-that self-crosslinking occurs in reaction system
Should.Self-crosslinking reaction can effectively improve the glass transition temperature of polymer, and substantial amounts of reaction system is consumed during self-crosslinking
, there is the phenomenon that oxidation turns yellow so as to reduce double bond glue spraying cotton fiber caused by by thermal cutoff in double bond.Additionally, small point of formaldehyde
Self-crosslinking reaction of the son in reaction system can also improve the bonding strength between emulsion and gum sprayed cotton, and be added significantly to emulsion
Dry film hardness.
2nd, in the high rigidity acrylate and vinyl acetate emulsion of high temperature resistant of the invention, color inhibition, the stronger emulsifier system of polarity is employed.
Itself and the bonding force between vinylacetate polar group are improved using the polarity of emulsifying agent, so as to effectively improve emulsion in high temperature
Stability under state.Also, polar group can play package action, activity on protection polymer molecular chain to polymer molecular chain
Larger group is not oxidized, the situation decomposed, aoxidize, turn yellow so as to avoid strand from occurring.
3rd, the high rigidity acrylate and vinyl acetate emulsion of high temperature resistant of the invention, color inhibition, using the preparation technology of the secondary dropwise addition of pre-emulsification.
The technique makes to form the stronger pre-emulsification environment of stability in reaction system, and it is anti-that follow-up emulsification is carried out while temperature is lifted
Should, so as to ensure that chemical reaction can thoroughly be carried out in reactor, improve the stability of emulsion itself.Additionally, in emulsion
The later stage of preparation introduces secondary oxidation, the rear elimination technique of reduction, and the technique can make the residual monomer dissociated during emulsion polymerization
Fully reacted, it is to avoid the generation of accessory substance, and improved the chemical stability of emulsion itself.
Specific embodiment
High temperature resistant of the invention, the high rigidity acrylate and vinyl acetate emulsion of color inhibition include water, butyl acrylate, vinylacetate, work(
Can monomer, N hydroxymethyl acrylamide, emulsifying agent, persulfate.Said components are calculated as according to mass fraction：100 parts of water, third
2-8 parts of olefin(e) acid butyl ester, vinylacetate 100-150 parts, function monomer 1-5 parts, N hydroxymethyl acrylamide 5-10 parts, emulsifying agent
1-5 parts, persulfate 0.1-1 parts.Long chain type acrylic acid reaction system can make to be difficult in the high temperature drying and shaping operation of gum sprayed cotton
Generation oxidation reaction, can avoid strand from the situation of pyrolytic occur.And N hydroxymethyl acrylamide under the high temperature conditions may be used
Formaldehyde small molecule is disengaged, and self-crosslinking reaction occurs in reaction system, sprayed caused by by thermal cutoff so as to reduce double bond
There is the phenomenon that oxidation turns yellow in collodion fiber.
High temperature resistant of the present invention, the function monomer of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are hydroxy-ethyl acrylate, acrylic acid hydroxyl
One kind in propyl ester, acrylic acid, itaconic acid is mixed with arbitrary proportion.First, hydroxy-ethyl acrylate has stronger cohesive
Can, rapid link of the gum sprayed cotton in shaping can be promoted.Secondly, hydroxypropyl acrylate except equally have relatively strong bond in addition to,
Also there is stronger weatherability and impact resistance, so as to the anti-yellowing property of glue spraying cotton fiber can be lifted.And acrylic acid then has
The fast advantage of reaction speed, and the double bond and carboxyl functional group association response of its high activity can be utilized, form the strand of crosslinking
Basic point, so as to improve the mechanical performance and bond properties of emulsion system.Finally, itaconic acid has unsaturated double-bond, and it is in reaction
There is stronger chemical reaction ability in system, and self-polymerization can be carried out and be polymerized with other monomers, so as to accelerate crosslinking mutual
Pass the formation of network molecular structure.
High temperature resistant of the present invention, the emulsifying agent of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are AEO, phosphoric acid half
One kind in ester ethoxylation disodium mixture is mixed with arbitrary proportion, and said components are respectively provided with the stronger group of polarity, its
Stronger interface activation ability itself is provided with, so as to can be shielded to polymer molecule chain structure, it is to avoid strand exists
Occurs the phenomenon that oxidation turns yellow under hot environment.
High temperature resistant of the present invention, the persulfate of the high rigidity acrylate and vinyl acetate emulsion of color inhibition use sodium peroxydisulfate, potassium peroxydisulfate, mistake
One kind or mentioned component in ammonium sulfate are mixed with arbitrary proportion.The Main Function of persulfate is to provide in the reaction freely
Base, makes it to produce the reaction such as free radical grafting, crosslinking with activated double bonds in reaction system, makes monomer be combined into certain sky
Between structure strand.
High temperature resistant of the present invention, the N hydroxymethyl acrylamide of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are effectively lived using 40-50%
Property component liquids, N hydroxymethyl acrylamide itself have stronger cross-linking properties, small point of formaldehyde can be disengaged under the high temperature conditions
Son is concurrently conigenous cross-linking reaction.And the control of N hydroxymethyl acrylamide concentration can be adjusted to reaction speed, to ensure breast
Change being smoothed out for reaction, and improve the stability of reaction system.
High temperature resistant of the present invention, the preparation method of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are comprised the following steps：
a）Raw material for standby is weighed according to said ratio；
b）30-40 parts of water, emulsifying agent, butyl acrylate, vinylacetate, function are added under normal temperature and pressure state in emulsion tank
Monomer and N hydroxymethyl acrylamide are simultaneously stirred well to uniform；
c）Excess water is added in a kettle., and temperature of reaction kettle is promoted to 65-70 DEG C, add the b step gained of 5-15% mixed
Compound, reacts 30-40 minutes；
d）Remaining b step gained mixture and persulfate is added dropwise toward step c gained mixture, reaction temperature is maintained at
75-80 DEG C and continue stirring, reaction time 3-5 hours；
e）80-85 DEG C is warming up to after Step d is added dropwise to complete, and is incubated 1-2 hours；
f）Obtain adding reductant-oxidant in mixture toward step e, be cooled to 70-75 DEG C, and be incubated 10-20 minutes；
g）Reductant-oxidant is added again toward mixture obtained in f steps, is cooled to 60-70 DEG C, and be incubated 10-20 minutes；
h）Mixture obtained in g steps is cooled to 40-50 DEG C, acrylic acid ester emulsion is obtained final product after filtering.
In the present invention, reductant-oxidant includes Oxidizing and Reducing Agents, and oxidant can use organic peroxide, and reduce
Agent can use vitamin C or sodium hydrogensulfite.The consumption of Oxidizing and Reducing Agents can consider addition according to being actually needed for reaction,
To ensure the stability of emulsion system after reacting.
Yellowing-resistant standard HG/T3689-2001 according to glue spraying cotton nonwoven fabrics determines, high temperature resistant of the invention, color inhibition
After 150 DEG C of high temperature drying and shapings of gum sprayed cotton, in standard A methods and B method testings, fiber is tried high rigidity acrylate and vinyl acetate emulsion
Sample is without there is xanthochromia.Tested according to gum sprayed cotton stiffness, 2X2cm needle punched carpets embryo cloth is soaked with emulsion of the present invention, and
Press dry after emulsion by 150 degree of drying, testing deflection with textile hard stiffness tester, its Ge Erlai deflection be more than
8000-10000mg。
It is described in detail with reference to a pair each embodiments of table, but does not therefore limit the invention to the implementation
In the range of example：
Embodiment 1
High temperature resistant of the invention, the high rigidity acrylate and vinyl acetate emulsion of color inhibition include water, butyl acrylate, vinylacetate, acrylic acid
Hydroxyl ethyl ester, N hydroxymethyl acrylamide, AEO, sodium peroxydisulfate.Said components are calculated as according to mass fraction：
100 parts of water, 2 parts of butyl acrylate, 100 parts of vinylacetate, 1 part of hydroxy-ethyl acrylate, 5 parts of N hydroxymethyl acrylamide, fat
1 part of fat alcohol APEO, 0.1 part of sodium peroxydisulfate.Wherein, N hydroxymethyl acrylamide is 40% effective active composition liquid.
High temperature resistant of the present invention, the preparation method of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are comprised the following steps：
a）Raw material for standby is weighed according to said ratio；
b）30 parts of water, emulsifying agent, butyl acrylate, vinylacetate, function lists are added under normal temperature and pressure state in emulsion tank
Body and N hydroxymethyl acrylamide are simultaneously stirred well to uniform；
c）Excess water is added in a kettle., and temperature of reaction kettle is promoted to 65 DEG C, add 5% b step gained mixture,
Reaction 30 minutes；
d）Remaining b step gained mixture and persulfate is added dropwise toward step c gained mixture, reaction temperature is maintained at 75
DEG C and continue stirring, 3 hours reaction time；
e）80 DEG C are warming up to after Step d is added dropwise to complete, and are incubated 1 hour；
f）Obtain adding reductant-oxidant in mixture toward step e, be cooled to 70 DEG C, and be incubated 10 minutes；
g）Reductant-oxidant is added again toward mixture obtained in f steps, is cooled to 60 DEG C, and be incubated 10 minutes；
h）Mixture obtained in g steps is cooled to 40 DEG C, acrylic acid ester emulsion is obtained final product after filtering.
In the present invention, reductant-oxidant includes Oxidizing and Reducing Agents, and oxidant can use organic peroxide, and reduce
Agent can use vitamin C or sodium hydrogensulfite.The consumption of Oxidizing and Reducing Agents can consider addition according to being actually needed for reaction,
To ensure the stability of emulsion system after reacting.
Yellowing-resistant standard HG/T3689-2001 according to glue spraying cotton nonwoven fabrics determines, high temperature resistant of the invention, color inhibition
After 150 DEG C of high temperature drying and shapings of gum sprayed cotton, in standard A methods and B method testings, fiber is tried high rigidity acrylate and vinyl acetate emulsion
Sample is without there is xanthochromia.Tested according to gum sprayed cotton stiffness, 2X2cm needle punched carpets embryo cloth is soaked with emulsion of the present invention, and
Press dry after emulsion by 150 degree of drying, testing deflection with textile hard stiffness tester, its Ge Erlai deflection be more than
8000mg。
Embodiment 2
High temperature resistant of the invention, the high rigidity acrylate and vinyl acetate emulsion of color inhibition include water, butyl acrylate, vinylacetate, acrylic acid
Hydroxyl ethyl ester, hydroxypropyl acrylate, acrylic acid, itaconic acid, N hydroxymethyl acrylamide, AEO, phosphoric acid half ester
Ethoxylation disodium, sodium peroxydisulfate, ammonium persulfate, potassium peroxydisulfate.Said components are calculated as according to mass fraction：100 parts of water, third
8 parts of olefin(e) acid butyl ester, 150 parts of vinylacetate, 1 part of hydroxy-ethyl acrylate, 1 part of hydroxypropyl acrylate, 2 parts of acrylic acid, itaconic acid 1
Part, 10 parts of N hydroxymethyl acrylamide, 2 parts of AEO, 3 parts of phosphoric acid half ester ethoxylation disodium, sodium peroxydisulfate
0.3 part, 0.3 part of ammonium persulfate, 0.4 part of potassium peroxydisulfate.Wherein, N hydroxymethyl acrylamide is 50% effective active composition liquid.
High temperature resistant of the present invention, the preparation method of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are comprised the following steps：
a）Raw material for standby is weighed according to said ratio；
b）40 parts of water, emulsifying agent, butyl acrylate, vinylacetate, function lists are added under normal temperature and pressure state in emulsion tank
Body and N hydroxymethyl acrylamide are simultaneously stirred well to uniform；
c）Excess water is added in a kettle., and temperature of reaction kettle is promoted to 70 DEG C, add 15% b step gained mixture,
Reaction 40 minutes；
d）Remaining b step gained mixture and persulfate is added dropwise toward step c gained mixture, reaction temperature is maintained at 80
DEG C and continue stirring, 5 hours reaction time；
e）85 DEG C are warming up to after Step d is added dropwise to complete, and are incubated 2 hours；
f）Obtain adding reductant-oxidant in mixture toward step e, be cooled to 75 DEG C, and be incubated 20 minutes；
g）Reductant-oxidant is added again toward mixture obtained in f steps, is cooled to 70 DEG C, and be incubated 20 minutes；
h）Mixture obtained in g steps is cooled to 50 DEG C, acrylic acid ester emulsion is obtained final product after filtering.
In the present invention, reductant-oxidant includes Oxidizing and Reducing Agents, and oxidant can use organic peroxide, and reduce
Agent can use vitamin C or sodium hydrogensulfite.The consumption of Oxidizing and Reducing Agents can consider addition according to being actually needed for reaction,
To ensure the stability of emulsion system after reacting.
Yellowing-resistant standard HG/T3689-2001 according to glue spraying cotton nonwoven fabrics determines, high temperature resistant of the invention, color inhibition
After 150 DEG C of high temperature drying and shapings of gum sprayed cotton, in standard A methods and B method testings, fiber is tried high rigidity acrylate and vinyl acetate emulsion
Sample is without there is xanthochromia.Tested according to gum sprayed cotton stiffness, 2X2cm needle punched carpets embryo cloth is soaked with emulsion of the present invention, and
Press dry after emulsion by 150 degree of drying, testing deflection with textile hard stiffness tester, its Ge Erlai deflection be more than
10000mg。
Embodiment 3
High temperature resistant of the invention, the high rigidity acrylate and vinyl acetate emulsion of color inhibition include water, butyl acrylate, vinylacetate, acrylic acid
Hydroxypropyl acrylate, acrylic acid, N hydroxymethyl acrylamide, phosphoric acid half ester ethoxylation disodium, ammonium persulfate.Said components are according to quality
Number is calculated as：100 parts of water, 4 parts of butyl acrylate, 120 parts of vinylacetate, 1 part of hydroxypropyl acrylate, 1 part of acrylic acid, N-
6 parts of NMA, 2 parts of phosphoric acid half ester ethoxylation disodium, 0.4 part of ammonium persulfate.Wherein, N hydroxymethyl acrylamide
It is 43% effective active composition liquid.
High temperature resistant of the present invention, the preparation method of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are comprised the following steps：
a）Raw material for standby is weighed according to said ratio；
b）34 parts of water, emulsifying agent, butyl acrylate, vinylacetate, function lists are added under normal temperature and pressure state in emulsion tank
Body and N hydroxymethyl acrylamide are simultaneously stirred well to uniform；
c）Excess water is added in a kettle., and temperature of reaction kettle is promoted to 66 DEG C, add 8% b step gained mixture,
Reaction 33 minutes；
d）Remaining b step gained mixture and persulfate is added dropwise toward step c gained mixture, reaction temperature is maintained at 76
DEG C and continue stirring, 3.5 hours reaction time；
e）81 DEG C are warming up to after Step d is added dropwise to complete, and are incubated 1 hour；
f）Obtain adding reductant-oxidant in mixture toward step e, be cooled to 71 DEG C, and be incubated 13 minutes；
g）Reductant-oxidant is added again toward mixture obtained in f steps, is cooled to 63 DEG C, and be incubated 13 minutes；
h）Mixture obtained in g steps is cooled to 43 DEG C, acrylic acid ester emulsion is obtained final product after filtering.
In the present invention, reductant-oxidant includes Oxidizing and Reducing Agents, and oxidant can use organic peroxide, and reduce
Agent can use vitamin C or sodium hydrogensulfite.The consumption of Oxidizing and Reducing Agents can consider addition according to being actually needed for reaction,
To ensure the stability of emulsion system after reacting.
Yellowing-resistant standard HG/T3689-2001 according to glue spraying cotton nonwoven fabrics determines, high temperature resistant of the invention, color inhibition
After 150 DEG C of high temperature drying and shapings of gum sprayed cotton, in standard A methods and B method testings, fiber is tried high rigidity acrylate and vinyl acetate emulsion
Sample is without there is xanthochromia.Tested according to gum sprayed cotton stiffness, 2X2cm needle punched carpets embryo cloth is soaked with emulsion of the present invention, and
Press dry after emulsion by 150 degree of drying, testing deflection with textile hard stiffness tester, its Ge Erlai deflection be more than
8500mg。
Embodiment 4
High temperature resistant of the invention, the high rigidity acrylate and vinyl acetate emulsion of color inhibition include water, butyl acrylate, vinylacetate, acrylic acid
Hydroxyl ethyl ester, acrylic acid, itaconic acid, N hydroxymethyl acrylamide, AEO, phosphoric acid half ester ethoxylation disodium,
Sodium peroxydisulfate, potassium peroxydisulfate.Said components are calculated as according to mass fraction：100 parts of water, 6 parts of butyl acrylate, vinylacetate
130 parts, 1 part of hydroxy-ethyl acrylate, 1 part of acrylic acid, 1 part of itaconic acid, 8 parts of N hydroxymethyl acrylamide, aliphatic alcohol polyethenoxy
2 parts of ether, 1 part of phosphoric acid half ester ethoxylation disodium, 0.3 part of sodium peroxydisulfate, 0.3 part of potassium peroxydisulfate.Wherein, N- methylols acryloyl
Amine is 46% effective active composition liquid.
High temperature resistant of the present invention, the preparation method of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are comprised the following steps：
a）Raw material for standby is weighed according to said ratio；
b）35 parts of water, emulsifying agent, butyl acrylate, vinylacetate, function lists are added under normal temperature and pressure state in emulsion tank
Body and N hydroxymethyl acrylamide are simultaneously stirred well to uniform；
c）Excess water is added in a kettle., and temperature of reaction kettle is promoted to 67 DEG C, add 11% b step gained mixture,
Reaction 36 minutes；
d）Remaining b step gained mixture and persulfate is added dropwise toward step c gained mixture, reaction temperature is maintained at 77
DEG C and continue stirring, 4 hours reaction time；
e）82 DEG C are warming up to after Step d is added dropwise to complete, and are incubated 1.5 hours；
f）Obtain adding reductant-oxidant in mixture toward step e, be cooled to 73 DEG C, and be incubated 16 minutes；
g）Reductant-oxidant is added again toward mixture obtained in f steps, is cooled to 66 DEG C, and be incubated 17 minutes；
h）Mixture obtained in g steps is cooled to 46 DEG C, acrylic acid ester emulsion is obtained final product after filtering.
In the present invention, reductant-oxidant includes Oxidizing and Reducing Agents, and oxidant can use organic peroxide, and reduce
Agent can use vitamin C or sodium hydrogensulfite.The consumption of Oxidizing and Reducing Agents can consider addition according to being actually needed for reaction,
To ensure the stability of emulsion system after reacting.
Yellowing-resistant standard HG/T3689-2001 according to glue spraying cotton nonwoven fabrics determines, high temperature resistant of the invention, color inhibition
After 150 DEG C of high temperature drying and shapings of gum sprayed cotton, in standard A methods and B method testings, fiber is tried high rigidity acrylate and vinyl acetate emulsion
Sample is without there is xanthochromia.Tested according to gum sprayed cotton stiffness, 2X2cm needle punched carpets embryo cloth is soaked with emulsion of the present invention, and
Press dry after emulsion by 150 degree of drying, testing deflection with textile hard stiffness tester, its Ge Erlai deflection be more than
9000mg。
Embodiment 5
High temperature resistant of the invention, the high rigidity acrylate and vinyl acetate emulsion of color inhibition include water, butyl acrylate, vinylacetate, acrylic acid
Hydroxyl ethyl ester, hydroxypropyl acrylate, acrylic acid, itaconic acid, N hydroxymethyl acrylamide, AEO, phosphoric acid half ester
Ethoxylation disodium, sodium peroxydisulfate, ammonium persulfate, potassium peroxydisulfate.Said components are calculated as according to mass fraction：100 parts of water, third
7 parts of olefin(e) acid butyl ester, 140 parts of vinylacetate, 1 part of hydroxy-ethyl acrylate, 1 part of hydroxypropyl acrylate, 1 part of acrylic acid, itaconic acid 1
Part, 9 parts of N hydroxymethyl acrylamide, 2 parts of AEO, 2 parts of phosphoric acid half ester ethoxylation disodium, sodium peroxydisulfate
0.2 part, 0.3 part of ammonium persulfate, 0.3 part of potassium peroxydisulfate.Wherein, N hydroxymethyl acrylamide is 48% effective active composition liquid.
High temperature resistant of the present invention, the preparation method of the high rigidity acrylate and vinyl acetate emulsion of color inhibition are comprised the following steps：
a）Raw material for standby is weighed according to said ratio；
b）38 parts of water, emulsifying agent, butyl acrylate, vinylacetate, function lists are added under normal temperature and pressure state in emulsion tank
Body and N hydroxymethyl acrylamide are simultaneously stirred well to uniform；
c）Excess water is added in a kettle., and temperature of reaction kettle is promoted to 69 DEG C, add 13% b step gained mixture,
Reaction 38 minutes；
d）Remaining b step gained mixture and persulfate is added dropwise toward step c gained mixture, reaction temperature is maintained at 79
DEG C and continue stirring, 4.5 hours reaction time；
e）84 DEG C are warming up to after Step d is added dropwise to complete, and are incubated 2 hours；
f）Obtain adding reductant-oxidant in mixture toward step e, be cooled to 74 DEG C, and be incubated 18 minutes；
g）Reductant-oxidant is added again toward mixture obtained in f steps, is cooled to 68 DEG C, and be incubated 19 minutes；
h）Mixture obtained in g steps is cooled to 48 DEG C, acrylic acid ester emulsion is obtained final product after filtering.
In the present invention, reductant-oxidant includes Oxidizing and Reducing Agents, and oxidant can use organic peroxide, and reduce
Agent can use vitamin C or sodium hydrogensulfite.The consumption of Oxidizing and Reducing Agents can consider addition according to being actually needed for reaction,
To ensure the stability of emulsion system after reacting.
Yellowing-resistant standard HG/T3689-2001 according to glue spraying cotton nonwoven fabrics determines, high temperature resistant of the invention, color inhibition
After 150 DEG C of high temperature drying and shapings of gum sprayed cotton, in standard A methods and B method testings, fiber is tried high rigidity acrylate and vinyl acetate emulsion
Sample is without there is xanthochromia.Tested according to gum sprayed cotton stiffness, 2X2cm needle punched carpets embryo cloth is soaked with emulsion of the present invention, and
Press dry after emulsion by 150 degree of drying, testing deflection with textile hard stiffness tester, its Ge Erlai deflection be more than
9500mg。
Claims (6)
1. the high rigidity acrylate and vinyl acetate emulsion of a kind of high temperature resistant, color inhibition, it is characterised in that：The high temperature resistant, the high rigidity of color inhibition
Acrylate and vinyl acetate emulsion includes water, butyl acrylate, vinylacetate, function monomer, N hydroxymethyl acrylamide, emulsifying agent, persulfuric acid
Salt, said components are calculated as according to mass fraction：100 parts of water, butyl acrylate 2-8 parts, vinylacetate 100-150 parts, work(
Can 1-5 parts, N hydroxymethyl acrylamide 5-10 parts, emulsifying agent 1-5 parts, persulfate 0.1-1 parts of monomer.
2. the high rigidity acrylate and vinyl acetate emulsion of high temperature resistant, color inhibition according to claim 1, it is characterised in that：The function monomer
Mix for the one kind in hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid, itaconic acid or with arbitrary proportion.
3. the high rigidity acrylate and vinyl acetate emulsion of high temperature resistant, color inhibition according to claim 1, it is characterised in that：The emulsifying agent is
One kind in AEO, phosphoric acid half ester ethoxylation disodium mixture is mixed with arbitrary proportion.
4. the high rigidity acrylate and vinyl acetate emulsion of high temperature resistant, color inhibition according to claim 1, it is characterised in that：Described persulfuric acid
Salt mixes for the one kind in sodium peroxydisulfate, ammonium persulfate, potassium peroxydisulfate or with arbitrary proportion.
5. the high rigidity acrylate and vinyl acetate emulsion of high temperature resistant, color inhibition according to claim 1, it is characterised in that：The N- methylols
Acrylamide is 40-50% effective active composition liquid.
6. a kind of high temperature resistant as claimed in claim 1, the preparation method of the high rigidity acrylate and vinyl acetate emulsion of color inhibition, it is characterised in that：
The preparation method is comprised the following steps：
a）Raw material for standby is weighed according to said ratio；
b）30-40 parts of water, emulsifying agent, butyl acrylate, vinylacetate, function are added under normal temperature and pressure state in emulsion tank
Monomer and N hydroxymethyl acrylamide are simultaneously stirred well to uniform；
c）Excess water is added in a kettle., and temperature of reaction kettle is promoted to 65-70 DEG C, add the b step gained of 5-15% mixed
Compound, reacts 30-40 minutes；
d）Remaining b step gained mixture and persulfate is added dropwise toward step c gained mixture, reaction temperature is maintained at
75-80 DEG C and continue stirring, reaction time 3-5 hours；
e）80-85 DEG C is warming up to after Step d is added dropwise to complete, and is incubated 1-2 hours；
f）Obtain adding reductant-oxidant in mixture toward step e, be cooled to 70-75 DEG C, and be incubated 10-20 minutes；
g）Reductant-oxidant is added again toward mixture obtained in f steps, is cooled to 60-70 DEG C, and be incubated 10-20 minutes；
h）Mixture obtained in g steps is cooled to 40-50 DEG C, acrylic acid ester emulsion is obtained final product after filtering.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107267095A (en) * | 2017-06-21 | 2017-10-20 | 合肥龙发包装有限公司 | A kind of beverage class carton adhesive |
| CN110093126A (en) * | 2019-03-27 | 2019-08-06 | 广州市永添生物科技有限公司 | A kind of preparation method of medical aqueous multiple emulsion paper-plastic lamination adhesive |
| CN113861901A (en) * | 2021-10-21 | 2021-12-31 | 湖北省宏源药业科技股份有限公司 | Modified polyvinyl acetate emulsion adhesive and preparation method thereof |
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| CN102863929A (en) * | 2012-09-17 | 2013-01-09 | 马千里 | Anti-yellowing emulsion polyacrylic ester pressure-sensitive adhesive and preparation method thereof |
| CN104558380A (en) * | 2014-12-23 | 2015-04-29 | 王新民 | Acrylic emulsion |
| CN105219290A (en) * | 2015-11-02 | 2016-01-06 | 天长市高新技术创业服务中心 | A kind of preparation method of anti-xanthochromia glazing film |
| CN105986479A (en) * | 2015-02-07 | 2016-10-05 | 福建鑫华股份有限公司 | Formula of yellowing-resistant polyvinyl acetate emulsion for fiber shoe insole and preparation method thereof |
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| CN102863929A (en) * | 2012-09-17 | 2013-01-09 | 马千里 | Anti-yellowing emulsion polyacrylic ester pressure-sensitive adhesive and preparation method thereof |
| CN104558380A (en) * | 2014-12-23 | 2015-04-29 | 王新民 | Acrylic emulsion |
| CN105986479A (en) * | 2015-02-07 | 2016-10-05 | 福建鑫华股份有限公司 | Formula of yellowing-resistant polyvinyl acetate emulsion for fiber shoe insole and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107267095A (en) * | 2017-06-21 | 2017-10-20 | 合肥龙发包装有限公司 | A kind of beverage class carton adhesive |
| CN110093126A (en) * | 2019-03-27 | 2019-08-06 | 广州市永添生物科技有限公司 | A kind of preparation method of medical aqueous multiple emulsion paper-plastic lamination adhesive |
| CN113861901A (en) * | 2021-10-21 | 2021-12-31 | 湖北省宏源药业科技股份有限公司 | Modified polyvinyl acetate emulsion adhesive and preparation method thereof |
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Application publication date: 20170613 |