CN110511315A - A kind of high barrier vinylidene chloride-acrylic acid ester emulsion and preparation method thereof - Google Patents
A kind of high barrier vinylidene chloride-acrylic acid ester emulsion and preparation method thereof Download PDFInfo
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- CN110511315A CN110511315A CN201910857451.XA CN201910857451A CN110511315A CN 110511315 A CN110511315 A CN 110511315A CN 201910857451 A CN201910857451 A CN 201910857451A CN 110511315 A CN110511315 A CN 110511315A
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- vinylidene chloride
- acrylic acid
- acid ester
- high barrier
- ester emulsion
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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
- C08F214/00—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 a halogen
- C08F214/02—Monomers containing chlorine
- C08F214/04—Monomers containing two carbon atoms
- C08F214/08—Vinylidene chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Polymerisation Methods In General (AREA)
Abstract
The present invention provides a kind of high barrier vinylidene chloride-acrylic acid ester emulsion and preparation method thereof, belongs to paint field.The lotion in parts by weight, including following component: 88~92 parts of vinylidene chloride, 8~12 parts of acrylic ester monomer, 1~1.5 part of initiator, 2.5~3.5 parts of emulsifier, 0.3~0.5 part of pH buffer.The present invention also provides a kind of preparation methods of high barrier vinylidene chloride-acrylic acid ester emulsion.Vinylidene chloride-acrylic acid ester emulsion of the invention has good barrier property and comprehensive performance.
Description
Technical field
The invention belongs to paint fields, and in particular to a kind of high barrier vinylidene chloride-acrylic acid ester emulsion and its preparation
Method.
Background technique
Vingon (abbreviation PVDC) is to be now widely used for one of important separated packaging material such as food, medicine.
In recent years, based on vinylidene chloride monomer synthesis lotion be free of inflammable and virose solvent, and film with it is good every
Oxygen waterproof performance, it can make packing material from the corrosion of oxygen, vapor, numerous soda acids and chemicals in environment.Except this it
Outside, there are also very strong toughness, high/low temperature tolerance and the performances such as printing are sealed using the membrane material of PVDC production, nearly 60 years
Carry out PVDC packaging material and applied packaging in food, military supplies, drug, pharmaceuticals etc. on a large scale, PVDC is in modern high resistant
Every also more and more being paid attention in packaging field.At the same time, it is " green " packaging material that PVDC material, which is also considered by industry,
Because the material utilization amount of PVDC packaging film will be greatly decreased compared to using market common packaging materials such as polyethylene, aluminium film etc., this
It can be reduced the waste of resource and the generation of waste, be finally reached the purpose of the utilization of resources and environmental protection two-win.But due to
Its thermal stability is poor, and leading to it, there are unmanageable defects, and introduces acrylate as comonomer, can be from reaction
Inside increase it is steady, then can the significantly stability of reinforced resin, barrier property, impart the more excellent performance of lotion.
CN104114585A discloses a kind of vinylidene chloride based copolymer lotion for blister package film, deficiency
Place is that impact strength is lower, synthesis technology is more complex, is unfavorable for producing.CN102876149A discloses a kind of coating self-adhesion
Property polyvinylidene emulsions and preparation method thereof, shortcoming is that thermal stability and yellowing-resistant ability are poor, so as to cause resistance
Separating performance reduces.
Summary of the invention
The purpose of the present invention is to solve the problems of existing polyvinylidene chloride copolymer lotion barrier property difference, and mention
For a kind of high barrier vinylidene chloride-acrylic acid ester emulsion and preparation method thereof.
To achieve the above object of the invention, it adopts the following technical scheme that:
Present invention firstly provides a kind of high barrier vinylidene chloride-acrylic acid ester emulsions, in parts by weight, including such as
Lower component:
Preferably, the acrylic ester monomer is methyl acrylate, butyl acrylate, Isooctyl acrylate monomer or first
The one or more of base methyl acrylate.
Preferably, the initiator is one of potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate and sodium hydrogensulfite
Or it is several.
Preferably, the initiator is the mixture that potassium peroxydisulfate and sodium hydrogensulfite are 4:1 according to mass ratio.
Preferably, the emulsifier is lauryl sodium sulfate, dodecyl sodium sulfate, neopelex
One or both of with OP-10.
Preferably, the emulsifier is the mixture that lauryl sodium sulfate and OP-10 are 3:1 according to mass ratio.
Preferably, the pH buffer is sodium carbonate.
The present invention also provides a kind of preparation methods of high barrier vinylidene chloride-acrylic acid ester emulsion, comprising the following steps:
(1) pre-emulsification: vinylidene, acrylic ester monomer, water, emulsifier and pH buffer being added into reaction kettle,
Mixed emulsion, the stirring of cracking pressure kettle are obtained, temperature is room temperature, and nitrogen purges 1~3min, and 30~60min of pre-emulsification is obtained pre-
Polymers；
(2) emulsion polymerization: initiator being added into reaction kettle, and closed reactor is warming up to 55~65 DEG C, and reaction 4~8 is small
When, obtain vinylidene chloride-acrylic acid ester emulsion.
Preferably, stirring rate is 140~160r/min in the step (1).
Preferably, the step (1) in mixed emulsion solid content be 40~50%.
Beneficial effects of the present invention
The present invention provides a kind of vinylidene chloride-acrylic acid ester emulsion, and the vinylidene chloride-acrylic acid ester emulsion is due to acrylic acid
The introducing of ester does pre-emulsification using suitable emulsifier, and control polymerization by rationally controlling the usage amount of acrylate monomer
In the process emulsifier, initiator, pH adjusting agent ratio and process conditions, the vinylidene chloride made-acrylic acid ester emulsion tool
There is good barrier property, while also improving the comprehensive performance of lotion, the present invention also provides a kind of vinylidene chloride-acrylate
The preparation method of lotion, the preparation method is simple, and the addition of organic solvent, not environmentally protective.
Specific embodiment
Below with reference to embodiment, the present invention is further described, following embodiments be it is illustrative, be not restrictive,
It cannot be limited the scope of protection of the present invention with following embodiments.
Present invention firstly provides a kind of vinylidene chloride-acrylic acid ester emulsions, according to parts by weight, comprising:
88~92 parts of vinylidene chloride, 8~12 parts of acrylic ester monomer, 1~1.5 part of initiator, emulsifier 2.5~3.5
Part, 0.3~0.5 part of pH buffer.
Acrylic ester monomer of the present invention preferably be selected from methyl acrylate, butyl acrylate, Isooctyl acrylate monomer and
The one or more of methyl methacrylate, total additional amount of acrylic ester monomer are the 8~12% of monomer total amount, preferably
10%,
Initiator of the present invention is preferably one in potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate and sodium hydrogensulfite
Kind is several, and more preferably potassium peroxydisulfate and sodium hydrogensulfite are the mixture of 4:1 according to mass ratio.
Emulsifier of the present invention is preferably lauryl sodium sulfate, dodecyl sodium sulfate, dodecyl benzene sulfonic acid
The mixture that one or both of sodium and OP-10, more preferably lauryl sodium sulfate and OP-10 are 3:1 according to mass ratio.
PH buffer of the present invention is preferably sodium carbonate.
The present invention also provides a kind of preparation methods of vinylidene chloride-acrylic acid ester emulsion, include the following:
(1) pre-emulsification: vinylidene, acrylic ester monomer, water, emulsifier, pH buffer are added into reaction kettle, obtains
To mixed emulsion, the solid content of the mixed emulsion is 40~50%；The stirring of cracking pressure kettle, the stirring rate are preferred
For 140~160r/min, temperature is room temperature, and nitrogen purges 1~3min, and 30~60min of pre-emulsification obtains prepolymer；
(2) emulsion polymerization: initiator being added into reaction kettle, and closed reactor is warming up to 55~65 DEG C, and reaction 4~8 is small
When, obtain vinylidene chloride-acrylic acid ester emulsion.
Further detailed description is done to the present invention below with reference to example.
Embodiment 1
(1) vinylidene chloride 135g, methyl acrylate 15g, water 225g, emulsifier 12 pre-emulsification: are added into reaction kettle
Sodium alkyl sulfate 3.375g, OP-10 1.125g, pH buffer sodium carbonate 0.6g, the solid content for controlling obtained lotion are
40%, cracking pressure kettle 150r/min stirring, temperature are room temperature, and nitrogen purges 2min, pre-emulsification 45min.
(2) emulsion polymerization: initiator potassium persulfate 1.5g, sodium hydrogensulfite 0.375g being added into reaction kettle, closed anti-
It answers kettle to be warming up to 60 DEG C, reacts 6 hours, high barrier vinylidene chloride-acrylic acid ester emulsion is made.
Vinylidene chloride-acrylic acid ester emulsion that embodiment 1 is prepared is tested for the property, and the results are shown in Table 1.
Embodiment 2
(1) vinylidene chloride 132g, butyl acrylate 18g, water 180g, emulsifier 12 pre-emulsification: are added into reaction kettle
Sodium alkyl sulfate 2.8g, OP-10 0.95g, pH buffer sodium carbonate 0.45g, the solid content for controlling obtained lotion is 45%,
Cracking pressure kettle 140r/min stirring, temperature are room temperature, and nitrogen purges 1min, pre-emulsification 30min.
(2) initiator potassium persulfate 1.2g, sodium hydrogensulfite 0.3g, confined reaction emulsion polymerization: are added into reaction kettle
Kettle is warming up to 55 DEG C, reacts 4 hours, and high barrier vinylidene chloride-acrylic acid ester emulsion is made.
Vinylidene chloride-acrylic acid ester emulsion that embodiment 2 is obtained is tested for the property, and the results are shown in Table 1.
Embodiment 3
(1) vinylidene chloride 138g, Isooctyl acrylate monomer 12g, water 150g, emulsifier ten pre-emulsification: are added into reaction kettle
Sodium dialkyl sulfate 3.9375g, OP-10 1.3125g, pH buffer sodium carbonate 0.75g control the solid content of obtained lotion
It is 50%, cracking pressure kettle 160r/min stirring, temperature is room temperature, and nitrogen purges 3min, pre-emulsification 60min.
(2) initiator potassium persulfate 1.8g, sodium hydrogensulfite 0.45g, confined reaction emulsion polymerization: are added into reaction kettle
Kettle is warming up to 65 DEG C, reacts 8 hours, and high barrier vinylidene chloride-acrylic acid ester emulsion is made.
Vinylidene chloride-acrylic acid ester emulsion that embodiment 3 is obtained is tested for the property, and the results are shown in Table 1.
Embodiment 4
(1) vinylidene chloride 135g, methyl methacrylate 15g, water 225g, emulsifier pre-emulsification: are added into reaction kettle
Lauryl sodium sulfate 3.375g, OP-10 1.125g, pH buffer sodium carbonate 0.6g, the solid content for controlling obtained lotion are
40%, cracking pressure kettle 150r/min stirring, temperature are room temperature, and nitrogen purges 1min, pre-emulsification 30min.
(2) emulsion polymerization: initiator potassium persulfate 1.5g, sodium hydrogensulfite 0.375g being added into reaction kettle, closed anti-
It answers kettle to be warming up to 60 DEG C, reacts 5 hours, high barrier vinylidene chloride-acrylic acid ester emulsion is made.
Vinylidene chloride-acrylic acid ester emulsion that embodiment 4 is obtained is tested for the property, and the results are shown in Table 1.
Comparative example 1
(1) vinylidene chloride 150g, water 225g, emulsifier sodium lauryl sulfate pre-emulsification: are added into reaction kettle
3.375g, OP-10 1.125g, pH buffer sodium carbonate 0.6g, the solid content for controlling obtained lotion is 40%, cracking pressure
Kettle 150r/min stirring, temperature are room temperature, and nitrogen purges 1min, pre-emulsification 30min.
(2) emulsion polymerization: initiator potassium persulfate 1.5g, sodium hydrogensulfite 0.375g being added into reaction kettle, closed anti-
It answers kettle to be warming up to 60 DEG C, reacts 5 hours, vinylidene chloride lotion is made.
The vinylidene chloride lotion that comparative example 1 obtains is tested for the property, the results are shown in Table 1.
Table 1
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.This technology is led
For the those of ordinary skill in domain, under the premise of not departing from of the invention separate, the present invention can also be made improvements and modifications,
These improvements and modifications also fall within the scope of protection of the claims of the present invention.
For the explanation of the disclosed embodiments, those skilled in the art may be implemented or using the present invention.It is right
The modification of above-described embodiment be to those skilled in the art it is easy to implement, principles defined herein can be not
In the case where departing from the scope of the present invention, realize in other embodiments.Therefore the present invention will be not only restricted to above-described embodiment, and
It is to meet principles disclosed herein and the consistent widest scope of feature.
Claims (10)
1. a kind of high barrier vinylidene chloride-acrylic acid ester emulsion, which is characterized in that in parts by weight, including such as the following group
Point:
2. a kind of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 1, which is characterized in that described
Acrylic ester monomer is one kind or several of methyl acrylate, butyl acrylate, Isooctyl acrylate monomer or methyl methacrylate
Kind.
3. a kind of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 1, which is characterized in that described
Initiator is one or more of potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate and sodium hydrogensulfite.
4. a kind of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 3, which is characterized in that described
Initiator is the mixture that potassium peroxydisulfate and sodium hydrogensulfite are 4:1 according to mass ratio.
5. a kind of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 1, which is characterized in that described
Emulsifier is one or both of lauryl sodium sulfate, dodecyl sodium sulfate, neopelex and OP-10.
6. a kind of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 1, which is characterized in that described
Emulsifier is the mixture that lauryl sodium sulfate and OP-10 are 3:1 according to mass ratio.
7. a kind of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 1, which is characterized in that the pH
Buffer is sodium carbonate.
8. a kind of preparation method of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 1, feature exist
In, comprising the following steps:
(1) pre-emulsification: vinylidene, acrylic ester monomer, water, emulsifier and pH buffer are added into reaction kettle, obtains
Mixed emulsion, the stirring of cracking pressure kettle, temperature are room temperature, and nitrogen purges 1~3min, and 30~60min of pre-emulsification obtains pre-polymerization
Object；
(2) emulsion polymerization: initiator being added into reaction kettle, and closed reactor is warming up to 55~65 DEG C, reacts 4~8 hours, obtains
To vinylidene chloride-acrylic acid ester emulsion.
9. a kind of preparation method of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 8, feature exist
In stirring rate is 140~160r/min in the step (1).
10. a kind of preparation method of high barrier vinylidene chloride-acrylic acid ester emulsion according to claim 8, feature
Be, the step (1) in mixed emulsion solid content be 40~50%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704689A (en) * | 2020-06-29 | 2020-09-25 | 天津城建大学 | High-adhesion water-based vinylidene chloride copolymer emulsion for metal surface and preparation method thereof |
| CN113024743A (en) * | 2021-03-08 | 2021-06-25 | 青海洁神环境能源产业有限公司 | Two-component PVDC latex for biological rotating disc |
| CN116769362A (en) * | 2023-06-21 | 2023-09-19 | 浙江衢州巨塑化工有限公司 | Preparation method of PVDC emulsion for medicine packaging |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109135450A (en) * | 2018-07-16 | 2019-01-04 | 天津市宝德包装有限公司 | A kind of food pack PVDC-MA high-barrier gluing and preparation method thereof |
| CN109438608A (en) * | 2018-11-07 | 2019-03-08 | 长春工业大学 | A kind of preparation method of degradable dinner set metachloroethylene copolymer water-based emulsion |
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2019
- 2019-09-11 CN CN201910857451.XA patent/CN110511315A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109135450A (en) * | 2018-07-16 | 2019-01-04 | 天津市宝德包装有限公司 | A kind of food pack PVDC-MA high-barrier gluing and preparation method thereof |
| CN109438608A (en) * | 2018-11-07 | 2019-03-08 | 长春工业大学 | A kind of preparation method of degradable dinner set metachloroethylene copolymer water-based emulsion |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704689A (en) * | 2020-06-29 | 2020-09-25 | 天津城建大学 | High-adhesion water-based vinylidene chloride copolymer emulsion for metal surface and preparation method thereof |
| CN111704689B (en) * | 2020-06-29 | 2022-04-26 | 天津城建大学 | High-adhesion water-based vinylidene chloride copolymer emulsion for metal surface and preparation method thereof |
| CN113024743A (en) * | 2021-03-08 | 2021-06-25 | 青海洁神环境能源产业有限公司 | Two-component PVDC latex for biological rotating disc |
| CN116769362A (en) * | 2023-06-21 | 2023-09-19 | 浙江衢州巨塑化工有限公司 | Preparation method of PVDC emulsion for medicine packaging |
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Application publication date: 20191129 |