CN108148215A - A kind of low-temperature heat-sealing EEA lotions and preparation method thereof - Google Patents
A kind of low-temperature heat-sealing EEA lotions and preparation method thereof Download PDFInfo
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- CN108148215A CN108148215A CN201711394118.7A CN201711394118A CN108148215A CN 108148215 A CN108148215 A CN 108148215A CN 201711394118 A CN201711394118 A CN 201711394118A CN 108148215 A CN108148215 A CN 108148215A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C08G81/021—Block or graft polymers containing only sequences of polymers of C08C or C08F
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2487/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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Abstract
A kind of low-temperature heat-sealing EEA lotions of the present invention are made by the heated pressurization emulsification of following components, and the proportioning of each component is as follows：70%~75% deionized water, 20%~25% ethylene ethyl acrylate copolymer (abbreviation EEA copolymers), 2%~5% acrylic copolymer, 1%~3% emulsifier, 0.5%~1.5%PH conditioning agents, 0.1%~0.2% antifoaming agent, 0.01%~0.05% initiator；The lotion is by adding in emulsifier, PH conditioning agents, initiator, antifoaming agent etc., temperature-pressure stirring is carried out in autoclave to emulsify EEA copolymers, since the emulsification and cross linked of EEA copolymers acts on, the EEA lotions with moderately good low-temperature heat-sealing performance are made；When the lotion envelope temperature is 65 DEG C, heat seal strength >=1.0N/15mm；Rise envelope temperature be 120 DEG C when, heat seal strength >=2.5N/15mm；The heat sealability and thermal stability of lotion are good, and the food high-speed for needing low-temperature heat-sealing especially suitable for candy, chocolate etc. is packed.
Description
Technical field
The present invention provides a kind of low-temperature heat-sealing lotion and preparation method thereof, belongs to novel environment friendly polymeric material field.
Background technology
Nowadays, as society constantly advances, great variety, such as sugar has occurred in the mode of production and life of people
The food of the heat sensitivitys such as fruit, chocolate needs high-speed packaging, and current packaging material low-temperature heat-sealing performance is poor, plays envelope temperature
Height can not meet the production requirement of present high-speed packaging.Patent CN103952096A is related to a kind of low-temperature hot-seal adhesive and preparation side
Method, the latex are made of following component raw material：VEA lotion 20-24, styrene-butadiene emulsion 12-14, propyl benzene lotion 18-20, acrylic acid 6-
8th, maleic anhydride 5-6, ethylene glycol 12-14, petroleum sodium sulfonate 1-2, aminopropyl triethoxysilane 4-6, vinylacetate
2-3, polyvinyl alcohol 2-3, diethanol amine 1-2, tert-butyl hydroperoxide 1-2, tackifying assistant 4-5, butyl acetate 40-50, the glue
The heat-sealing temperature of breast is 105 DEG C.The high barrier food package coated membrane latexes by thermal sealing at low temperature and system that patent CN101358054 is related to
Preparation Method, the monomer which uses include vinylidene chloride and account for the 80-93% of mix monomer total amount, methyl acrylate, ethyl ester,
Methyl methacrylate, butyl ester, acrylonitrile or methacrylonitrile account for the 2-10% of mix monomer total amount, itaconic acid, acrylic acid, first
Base acrylic acid accounts for the 0.5-5% of mix monomer total amount, and the preparation method of the latex is using a polymerization, the heat-sealing of the latex
Temperature is 100 DEG C.The heat-sealing temperature of latex is 100 DEG C or more proposed in two above patent, and envelope temperature is higher, to sugar
The destruction of the heat sensitivitys food such as fruit, chocolate is larger, it is impossible to meet the requirement of high-speed packaging.In order to solve these problems, originally
Invention prepares a kind of low-temperature heat-sealing EEA lotions, under relatively low heat-sealing temperature, reaches same heat sealability.
Invention content
The present invention provides a kind of low-temperature heat-sealing EEA lotions, and the lotion is by adding in emulsifier, PH conditioning agents, initiator, disappearing
Infusion etc. carries out temperature-pressure stirring to emulsify EEA copolymers, due to the emulsification and cross linked of EEA copolymers in autoclave
The EEA lotions with moderately good low-temperature heat-sealing performance are made in effect；When the lotion envelope temperature is 65 DEG C, heat seal strength >=
1.0N/15mm；Rise envelope temperature be 120 DEG C when, heat seal strength >=2.5N/15mm；The heat sealability and thermal stability of lotion are good
Good, the food high-speed for needing low-temperature heat-sealing especially suitable for candy, chocolate etc. is packed.
A kind of low-temperature heat-sealing EEA lotions are made by the heated pressurization emulsification of following components, and the proportioning of each component is as follows：
70%~75% deionized water, 20%~25% ethylene-ethyl acrylate copolymer (abbreviation EEA copolymers), 2%~5% the third
Olefin(e) acid copolymer, 1%~3% emulsifier, 0.5%~1.5%pH conditioning agents, 0.1%~0.2% antifoaming agent, 0.01%~
0.05% initiator；
The melt index of the EEA copolymers is 200g/10min；
The glass transition temperature of the acrylic copolymer is 70 DEG C；
The emulsifier is polyacrylamide amine emulsifier；
The pH adjusting agent is commercially available ammonium hydroxide；
The antifoaming agent is polyoxyethylene polyoxypropylene pentaerythrite ether；
The initiator is tert-butyl hydroperoxide.
The present invention also provides a kind of preparation methods of above-mentioned low-temperature heat-sealing lotion, include the following steps：
(1) configuration of emulsifier
The emulsifier and appropriate amount of deionized water for weighing 1%~3% mix, and heat and stir 1h, heating temperature for 50~
60 DEG C, stir speed (S.S.) is 100~180r/min, spare.
(2) preparation of lotion
Sequentially added in high-temperature high-pressure reaction kettle remaining deionized water, 20%~25%EEA copolymers and 2%~
5% acrylic copolymer, stir speed (S.S.) are 300~500r/min；The prepared emulsifier in the first step is added in, passes through pumping
The mode of vacuum nitrogen gas replaces gas reactor 3 times, and then continuing to be filled with nitrogen makes reaction under high pressure reach the pressure in kettle
1.5Mpa adjusts mixing speed to 1500r/min, is heated to 100 DEG C, 3~5h of constant temperature, adds in 0.5%~1.5%pH tune again
Agent, 0.1~0.2% antifoaming agent and 0.01%~0.05% initiator are saved, mixing speed is 100~180r/min；Treat reaction knot
Shu Hou, autoclave are down to room temperature, filter out impurity, obtain low-temperature heat-sealing EEA lotions.
Low-temperature heat-sealing EEA lotions of the present invention, after being coated on PET or BOPP film, coating weight is 2.0~3.0g/m2, 40 DEG C
Cure 48h, test coated rear film heat sealability：When heat-sealing temperature is 65 DEG C, heat seal strength >=1.0N/15mm；Heat-sealing temperature
When being 120 DEG C, heat seal strength >=2.5N/15mm；Adhesive force is preferable simultaneously, under the prolonged condition of high temperature, the viscosity of lotion
It is kept with thermal stability good.
Specific embodiment
Embodiment one：
70% deionized water
25%EEA copolymers
2% acrylic copolymer
2% emulsifier
0.75%PH conditioning agents
0.2% antifoaming agent
0.05% initiator
1) configuration of emulsifier
The mixing of 2g polyacrylamide 15g deionized waters is weighed, 52 DEG C is heated to, heats and stir 1h, heating temperature 50
DEG C, stir speed (S.S.) 110r/min is spare.
2) preparation of lotion
It is sequentially added in high-temperature high-pressure reaction kettle：Deionized water 55g, 25gEEA copolymer, the acrylic copolymer of 2g,
Stir speed (S.S.) is 300r/min.The prepared emulsifier in the first step is added in, kettle is replaced by way of vacuum nitrogen gas
Interior gas 3 times, then continuing to be filled with nitrogen makes reaction under high pressure that the pressure in kettle be made to reach 1.5Mpa, adjust mixing speed to
1500r/min is heated to 100 DEG C, 3~5h of constant temperature, adds in 0.75g pH adjusting agents, 0.2g antifoaming agent, 0.05g again and causes
Agent, mixing speed 110r/min.It treats that after reaction, autoclave is down to room temperature, filters out impurity and obtain the low of the present invention
Warm envelope lotion.
3) coating machine coating lotion
Using BOPP film as base material, coating machine is coated with low-temperature heat-sealing lotion obtained above, coating weight 2.1g/m2, 40
DEG C curing 48h.Survey the film heat sealability of coating：When heat-sealing temperature is 65 DEG C, strong 1.2N/15mm is sealed；Heat-sealing temperature is 120
DEG C when, heat seal strength 2.5N/15mm.
Embodiment two：
73% deionized water
23%EEA copolymers
2% acrylic copolymer
1% emulsifier
0.8%PH conditioning agents
0.15% antifoaming agent
0.05% initiator
1) configuration of emulsifier
The mixing of 10g polyacrylamide 130g deionized waters is weighed, 55 DEG C is heated to, heats and stir 1h, heating temperature is
It is 50 DEG C, stir speed (S.S.) 120r/min, spare.
2) preparation of lotion
It is sequentially added in high-temperature high-pressure reaction kettle：Deionized water 600g, 230gEEA copolymer, the acrylic acid copolymer of 20g
Object, stir speed (S.S.) 300r/min.The prepared emulsifier in the first step is added in, is replaced by way of vacuum nitrogen gas
Gas reactor 3 times, then continuing to be filled with nitrogen makes reaction under high pressure that the pressure in kettle be made to reach 1.5Mpa, adjust mixing speed to
1500r/min is heated to 100 DEG C, 3~5h of constant temperature, adds in 8g pH adjusting agents, 1.5g antifoaming agent, 0.5g initiators again, stirs
Speed is mixed as 120r/min.It treats that after reaction, autoclave is down to room temperature, filters out impurity and obtain the low-temperature heat-sealing of the present invention
Lotion.
3) coating machine coating lotion
Using BOPP film as base material, coating machine is coated with low-temperature heat-sealing lotion obtained above, coating weight 2.0g/m2, 40
DEG C curing 48h.Survey the film heat sealability of coating：When heat-sealing temperature is 65 DEG C, strong 1.1N/15mm is sealed；Heat-sealing temperature is 120
DEG C when, heat seal strength 2.6N/15mm.
Embodiment three：
72% deionized water
23%EEA copolymers
2% acrylic copolymer
2% emulsifier
0.8%PH conditioning agents
0.17% antifoaming agent
0.03% initiator
1) configuration of emulsifier
The mixing of 2g polyacrylamide 12g deionized waters is weighed, 55 DEG C is heated to, heats and stir 1h, heating temperature 50
DEG C, stir speed (S.S.) 140r/min is spare.
2) preparation of lotion
It is sequentially added in high-temperature high-pressure reaction kettle：Deionized water 60g, 23gEEA copolymer, the acrylic copolymer of 2g,
Stir speed (S.S.) is 300r/min.The prepared emulsifier in the first step is added in, kettle is replaced by way of vacuum nitrogen gas
Interior gas 3 times, then continuing to be filled with nitrogen makes reaction under high pressure that the pressure in kettle be made to reach 1.5Mpa, adjust mixing speed to
1500r/min is heated to 100 DEG C, 3~5h of constant temperature, adds in 0.8g pH adjusting agents, 0.17g antifoaming agent, 0.03g again and causes
Agent, mixing speed 130r/min.It treats that after reaction, autoclave is down to room temperature, filters out impurity and obtain the low of the present invention
Warm envelope lotion.
3) coating machine coating lotion
Using BOPP film as base material, coating machine is coated with low-temperature heat-sealing lotion obtained above, coating weight 2.2g/m2, 40
DEG C curing 48h.Survey the film heat sealability of coating：When heat-sealing temperature is 65 DEG C, strong 1.2N/15mm is sealed；Heat-sealing temperature is 120
DEG C when, heat seal strength 2.6N/15mm.
Example IV：
70% deionized water
25%EEA copolymers
3% acrylic copolymer
1% emulsifier
0.85%PH conditioning agents
0.1% antifoaming agent
0.05% initiator
1) configuration of emulsifier
The mixing of 1g polyacrylamide 10g deionized waters is weighed, 56 DEG C is heated to, heats and stir 1h, heating temperature 50
DEG C, stir speed (S.S.) 150r/min is spare.
2) preparation of lotion
It is sequentially added in high-temperature high-pressure reaction kettle：Deionized water 60g, 25gEEA copolymer, the acrylic copolymer of 3g,
Stir speed (S.S.) is 300r/min.The prepared emulsifier in the first step is added in, kettle is replaced by way of vacuum nitrogen gas
Interior gas 3 times, then continuing to be filled with nitrogen makes reaction under high pressure that the pressure in kettle be made to reach 1.5Mpa, adjust mixing speed to
1500r/min is heated to 100 DEG C, 3~5h of constant temperature, adds in 0.85g pH adjusting agents, 0.1g antifoaming agent, 0.05g again and causes
Agent, mixing speed 150r/min.It treats that after reaction, autoclave is down to room temperature, filters out impurity and obtain the low of the present invention
Warm envelope lotion.
3) coating machine coating lotion
Using BOPP film as base material, coating machine is coated with low-temperature heat-sealing lotion obtained above, coating weight 2.1g/m2, 40
DEG C curing 48h.Survey the film heat sealability of coating：When heat-sealing temperature is 65 DEG C, strong 1.1N/15mm is sealed；Heat-sealing temperature is 120
DEG C when, heat seal strength 2.7N/15mm.
Embodiment five：
70% deionized water
25%EEA copolymers
2% acrylic copolymer
2% emulsifier
0.75%PH conditioning agents
0.2% antifoaming agent
0.05% initiator
1) configuration of emulsifier
The mixing of 2g polyacrylamide 15g deionized waters is weighed, 58 DEG C is heated to, heats and stir 1h, heating temperature 50
DEG C, stir speed (S.S.) 160r/min is spare.
2) preparation of lotion
It is sequentially added in high-temperature high-pressure reaction kettle：Deionized water 55g, 25gEEA copolymer, the acrylic copolymer of 2g,
Stir speed (S.S.) is 300r/min.The prepared emulsifier in the first step is added in, kettle is replaced by way of vacuum nitrogen gas
Interior gas 3 times, then continuing to be filled with nitrogen makes reaction under high pressure that the pressure in kettle be made to reach 1.5Mpa, adjust mixing speed to
1500r/min is heated to 100 DEG C, 3~5h of constant temperature, adds in 0.75g pH adjusting agents, 0.2g antifoaming agent, 0.05g again and causes
Agent, mixing speed 160r/min.It treats that after reaction, autoclave is down to room temperature, filters out impurity and obtain the low of the present invention
Warm envelope lotion.
3) coating machine coating lotion
Using BOPP film as base material, coating machine is coated with low-temperature heat-sealing lotion obtained above, coating weight 2.1g/m2, 40
DEG C curing 48h.Survey the film heat sealability of coating：When heat-sealing temperature is 65 DEG C, strong 1.2N/15mm is sealed；Heat-sealing temperature is 120
DEG C when, heat seal strength 2.7N/15mm.
Embodiment six：
75% deionized water
21%EEA copolymers
2% acrylic copolymer
1% emulsifier
0.76%PH conditioning agents
0.2% antifoaming agent
0.04% initiator
1) configuration of emulsifier
The mixing of 10g polyacrylamide 140g deionized waters is weighed, 60 DEG C is heated to, heats and stir 1h, heating temperature is
It is 50 DEG C, stir speed (S.S.) 180r/min, spare.
2) preparation of lotion
It is sequentially added in high-temperature high-pressure reaction kettle：Deionized water 610g, 210gEEA copolymer, the acrylic acid copolymer of 20g
Object, stir speed (S.S.) 300r/min.The prepared emulsifier in the first step is added in, is replaced by way of vacuum nitrogen gas
Gas reactor 3 times, then continuing to be filled with nitrogen makes reaction under high pressure that the pressure in kettle be made to reach 1.5Mpa, adjust mixing speed to
1500r/min is heated to 100 DEG C, 3~5h of constant temperature, adds in 7.6g pH adjusting agents, 2g antifoaming agent, 0.4g initiators again, stirs
Speed is mixed as 180r/min.It treats that after reaction, autoclave is down to room temperature, filters out impurity and obtain the low-temperature heat-sealing of the present invention
Lotion.
3) coating machine coating lotion
Using BOPP film as base material, coating machine is coated with low-temperature heat-sealing lotion obtained above, coating weight 2.0g/m2, 40
DEG C curing 48h.Survey the film heat sealability of coating：When heat-sealing temperature is 65 DEG C, strong 1.1N/15mm is sealed；Heat-sealing temperature is 120
DEG C when, heat seal strength 2.7N/15mm.
Claims (9)
1. a kind of low-temperature heat-sealing EEA lotions, which is characterized in that the lotion is made by following components：70%~75% deionized water,
20%~25%EEA copolymers, 2%~5% acrylic copolymer, 1%~3% emulsifier, 0.5%~1.5%pH conditioning agents,
0.1%~0.2% antifoaming agent, 0.01%~0.05% initiator.
2. low-temperature heat-sealing EEA lotions according to claim 1, which is characterized in that the ethylene-ethyl acrylate copolymer
Melt index be 200g/10min.
3. low-temperature heat-sealing EEA lotions according to claim 1, which is characterized in that the vitrifying of the acrylic copolymer
Temperature is 70 DEG C.
4. low-temperature heat-sealing EEA lotions according to claim 1, which is characterized in that the emulsifier is polyacrylamide breast
Agent.
5. low-temperature heat-sealing EEA lotions according to claim 1, which is characterized in that the antifoaming agent is polyoxyethylene polyoxy
Propylene pentaerythrite ether.
6. low-temperature heat-sealing EEA lotions according to claim 1, which is characterized in that the initiator is tert-butyl hydroperoxide
Hydrogen.
7. according to the preparation method of any low-temperature heat-sealing EEA lotions of claim 1-6, which is characterized in that it include with
Lower step：
(1) configuration of emulsifier
The emulsifier and appropriate amount of deionized water for weighing 1%~3% mix, and heat and stir 1h, and heating temperature is 50~60 DEG C,
Stir speed (S.S.) is 100~180r/min；
(2) preparation of lotion
Remaining deionized water, 20%~25%EEA copolymers and 2%~5% are sequentially added in high-temperature high-pressure reaction kettle
Acrylic copolymer, stir speed (S.S.) are 300~500r/min；The prepared emulsifier in the first step is added in, by vacuumizing
The mode of inflated with nitrogen replaces gas reactor 3 times, and then continuing to be filled with nitrogen makes reaction under high pressure that the pressure in kettle be made to reach 1.5Mpa,
Mixing speed is adjusted to 1500r/min, is heated to 100 DEG C, 3~5h of constant temperature, add in again 0.5%~1.5%pH conditioning agents,
0.1~0.2% antifoaming agent and 0.01%~0.05% initiator, mixing speed are 100~180r/min；It treats after reaction,
Autoclave is down to room temperature, filters out impurity, obtains low-temperature heat-sealing EEA lotions.
8. the application of low-temperature heat-sealing EEA lotions according to claim 1, which is characterized in that the lotion is used for film.
9. a kind of coated thin film, which is characterized in that be made by low-temperature heat-sealing EEA lotions described in claim 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020214257A1 (en) | 2019-04-17 | 2020-10-22 | Dow Global Technologies Llc | Waterborne dispersion composition |
| WO2022233095A1 (en) * | 2021-05-06 | 2022-11-10 | 海南必凯水性新材料有限公司 | Special heat-sealing emulsion for kraft paper and preparation method therefor |
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| CN103059213A (en) * | 2012-12-26 | 2013-04-24 | 海南必凯水性涂料有限公司 | Low-temperature heat-seal acrylic emulsion and preparation method thereof and application thereof |
| CN105482740A (en) * | 2015-12-27 | 2016-04-13 | 吴姣 | Hot melt adhesive |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100056696A1 (en) * | 2008-09-02 | 2010-03-04 | Poole Elizabeth A | Low emission, high scrub VAE latex Paints |
| CN102286257A (en) * | 2011-06-16 | 2011-12-21 | 上海邦中高分子材料有限公司 | Special high temperature resistant adhesive resins for steel-plastic composite pipe and preparation method thereof |
| CN102850891A (en) * | 2012-09-09 | 2013-01-02 | 海南必凯水性涂料有限公司 | Low-temperature heat-seal acrylic emulsion for coating and preparation method thereof |
| CN103059213A (en) * | 2012-12-26 | 2013-04-24 | 海南必凯水性涂料有限公司 | Low-temperature heat-seal acrylic emulsion and preparation method thereof and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020214257A1 (en) | 2019-04-17 | 2020-10-22 | Dow Global Technologies Llc | Waterborne dispersion composition |
| WO2022233095A1 (en) * | 2021-05-06 | 2022-11-10 | 海南必凯水性新材料有限公司 | Special heat-sealing emulsion for kraft paper and preparation method therefor |
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