CN106084119A - A kind of acrylic resin and preparation method thereof - Google Patents

A kind of acrylic resin and preparation method thereof Download PDF

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Publication number
CN106084119A
CN106084119A CN201610730897.2A CN201610730897A CN106084119A CN 106084119 A CN106084119 A CN 106084119A CN 201610730897 A CN201610730897 A CN 201610730897A CN 106084119 A CN106084119 A CN 106084119A
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CN
China
Prior art keywords
parts
resin
aqueous phase
reaction system
acrylic resin
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Application number
CN201610730897.2A
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Chinese (zh)
Inventor
李毅
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Individual
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Individual
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Priority to CN201610730897.2A priority Critical patent/CN106084119A/en
Publication of CN106084119A publication Critical patent/CN106084119A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/14Methyl esters, e.g. methyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/12Polymerisation in non-solvents
    • C08F2/16Aqueous medium
    • C08F2/20Aqueous medium with the aid of macromolecular dispersing agents

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The present invention relates to a kind of acrylic resin and preparation method thereof, belong to acrylic resin technical field.The present invention includes following raw materials by weight: oil phase: methyl methacrylate 30 40 parts, acrylonitrile 5 10 parts, lauryl acrylate 35 parts, butyl acrylate 5 10 parts, azodiisobutyronitrile 13 parts;Aqueous phase: polyvinyl alcohol 35 parts, 5 10 parts of gelatin, NaCl10 20 parts, CaCO35 parts, deionized water 500 parts.The present invention uses environmentally-friendly technique process for suspension polymerization, with methyl methacrylate as primary raw material, by adding the monomers such as acrylonitrile, lauryl acrylate, butyl acrylate, with azodiisobutyronitrile (AIBN) as initiator, it is prepared for a kind of high-performance acrylic acid resin.This resin is in addition to can be used for the biomedical materials such as dentistry, it may also be used for the fields such as high grade paint.

Description

A kind of acrylic resin and preparation method thereof
Technical field
The present invention relates to a kind of resin and preparation method thereof, it is more particularly related to a kind of acrylic resin and Its preparation method, belongs to acrylic resin technical field.
Background technology
Acrylic resin has that color is shallow, transparency is high, bright plentiful, film is tough and tensile, adhesive force is strong, the feature such as corrosion-resistant, It it is conventional coating material.Owing to acrylic resin exists certain defect in specific occasion, such as hardness, resistance tocrocking, resistance to molten Agent, mechanical performance be the best and high expensive etc., limits its further application.In recent years, along with polymerization technique Constantly improve and development, and acrylic resin combination property requirement is improved constantly, people's weight to environment-friendly products in addition Depending on, use environmentally-friendly technique to prepare high-performance acrylic acid resin and get more and more people's extensive concerning.
Summary of the invention
Present invention seek to address that prior art prepares the environment of acrylic resin the most friendly, the highest the asking of properties of product Topic, it is provided that a kind of acrylic resin, the preparation environmental friendliness of this resin, performance is higher.
In order to realize foregoing invention purpose, its concrete technical scheme is as follows:
A kind of acrylic resin, it is characterised in that: include following raw materials by weight:
Oil phase:
Methyl methacrylate 30-40 part
Acrylonitrile 5-10 part
Lauryl acrylate 3-5 part
Butyl acrylate 5-10 part
Azodiisobutyronitrile 1-3 part
Aqueous phase:
Polyvinyl alcohol 3-5 part
Gelatin 5-10 part
NaCl 10-20 part
CaCO35 parts
Deionized water 500 parts.
A kind of preparation method of acrylic resin, it is characterised in that: comprise the following steps that:
A, accurately weigh each raw material in oil phase according to recipe requirements and be sufficiently mixed uniformly in container, standby;
B, according to aqueous phase recipe requirements, each raw material is added in a tool stirring, condensing tube and charge door there-necked flask;By system temperature Rise to 30-50 DEG C, start stirring until each component is sufficiently mixed dissolving;
C, oil mixture step A prepared are poured in the aqueous phase there-necked flask that step B prepares;Keep reactor stirs Speed be 200-300 rev/min, make oil phase form uniform bead and be dispersed in the aqueous phase prepared in advance;It is warming up to 72- 76 DEG C, until bead sizing;
D, polymerization reaction system temperature is raised to 80 DEG C, insulation 2-3 hour;Polymerization reaction system is warming up to 85 DEG C, insulation 2-3 hour;Polymerization reaction system is warming up to 90 DEG C, insulation 2-3 hour;Reaction system is cooled to 30-50 DEG C, leaches Resin bead;
E, employing ethanol carry out drip washing to resin, and the impurity of removing resin air-dries and i.e. obtains polyacrylic resin.
The Advantageous Effects that the present invention brings:
The present invention uses environmentally-friendly technique process for suspension polymerization, with methyl methacrylate as primary raw material, by adding third The monomers such as alkene nitrile, lauryl acrylate, butyl acrylate, with azodiisobutyronitrile (AIBN) as initiator, are prepared for a kind of high Performance acrylic resin.This resin is in addition to can be used for the biomedical materials such as dentistry, it may also be used for the fields such as high grade paint.
Detailed description of the invention
Embodiment 1
A kind of acrylic resin, including following raw materials by weight:
Oil phase:
Methyl methacrylate 30 parts
Acrylonitrile 5 parts
Lauryl acrylate 3 parts
Butyl acrylate 5 parts
Azodiisobutyronitrile 1 part
Aqueous phase:
Polyvinyl alcohol 3 parts
5 parts of gelatin
NaCl 10 parts
CaCO35 parts
Deionized water 500 parts.
Embodiment 2
A kind of acrylic resin, including following raw materials by weight:
Oil phase:
Methyl methacrylate 40 parts
Acrylonitrile 10 parts
Lauryl acrylate 5 parts
Butyl acrylate 10 parts
Azodiisobutyronitrile 3 parts
Aqueous phase:
Polyvinyl alcohol 5 parts
10 parts of gelatin
NaCl 20 parts
CaCO35 parts
Deionized water 500 parts.
Embodiment 3
A kind of acrylic resin, including following raw materials by weight:
Oil phase:
Methyl methacrylate 35 parts
Acrylonitrile 7.5 parts
Lauryl acrylate 4 parts
Butyl acrylate 7.5 parts
Azodiisobutyronitrile 2 parts
Aqueous phase:
Polyvinyl alcohol 4 parts
7.5 parts of gelatin
NaCl 15 parts
CaCO35 parts
Deionized water 500 parts.
Embodiment 4
A kind of acrylic resin, including following raw materials by weight:
Oil phase:
Methyl methacrylate 32 parts
Acrylonitrile 9 parts
Lauryl acrylate 3.5 parts
Butyl acrylate 8 parts
Azodiisobutyronitrile 1.2 parts
Aqueous phase:
Polyvinyl alcohol 3.5 parts
6.5 parts of gelatin
NaCl 11 parts
CaCO35 parts
Deionized water 500 parts.
Embodiment 5
A, accurately weigh each raw material in oil phase according to recipe requirements and be sufficiently mixed uniformly in container, standby;
B, according to aqueous phase recipe requirements, each raw material is added in a tool stirring, condensing tube and charge door there-necked flask;By system temperature Rise to 30 DEG C, start stirring until each component is sufficiently mixed dissolving;
C, oil mixture step A prepared are poured in the aqueous phase there-necked flask that step B prepares;Keep reactor stirs Speed be 200 revs/min, make oil phase form uniform bead and be dispersed in the aqueous phase prepared in advance;It is warming up to 72 DEG C, directly Shape to bead;
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 2 hours;Polymerization reaction system is warming up to 85 DEG C, is incubated 2 Hour;Polymerization reaction system is warming up to 90 DEG C, is incubated 2 hours;Reaction system is cooled to 30 DEG C, leaches resin bead;
E, employing ethanol carry out drip washing to resin, and the impurity of removing resin air-dries and i.e. obtains polyacrylic resin.
Embodiment 6
A, accurately weigh each raw material in oil phase according to recipe requirements and be sufficiently mixed uniformly in container, standby;
B, according to aqueous phase recipe requirements, each raw material is added in a tool stirring, condensing tube and charge door there-necked flask;By system temperature Rise to 50 DEG C, start stirring until each component is sufficiently mixed dissolving;
C, oil mixture step A prepared are poured in the aqueous phase there-necked flask that step B prepares;Keep reactor stirs Speed be 300 revs/min, make oil phase form uniform bead and be dispersed in the aqueous phase prepared in advance;It is warming up to 76 DEG C, directly Shape to bead;
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 3 hours;Polymerization reaction system is warming up to 85 DEG C, is incubated 3 Hour;Polymerization reaction system is warming up to 90 DEG C, is incubated 3 hours;Reaction system is cooled to 50 DEG C, leaches resin bead;
E, employing ethanol carry out drip washing to resin, and the impurity of removing resin air-dries and i.e. obtains polyacrylic resin.
Embodiment 7
A, accurately weigh each raw material in oil phase according to recipe requirements and be sufficiently mixed uniformly in container, standby;
B, according to aqueous phase recipe requirements, each raw material is added in a tool stirring, condensing tube and charge door there-necked flask;By system temperature Rise to 40 DEG C, start stirring until each component is sufficiently mixed dissolving;
C, oil mixture step A prepared are poured in the aqueous phase there-necked flask that step B prepares;Keep reactor stirs Speed be 250 revs/min, make oil phase form uniform bead and be dispersed in the aqueous phase prepared in advance;It is warming up to 74 DEG C, directly Shape to bead;
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 2.5 hours;Polymerization reaction system is warming up to 85 DEG C, insulation 2.5 hours;Polymerization reaction system is warming up to 90 DEG C, is incubated 2.5 hours;Reaction system is cooled to 40 DEG C, leaches tree Fat bead;
E, employing ethanol carry out drip washing to resin, and the impurity of removing resin air-dries and i.e. obtains polyacrylic resin.
Embodiment 8
A, accurately weigh each raw material in oil phase according to recipe requirements and be sufficiently mixed uniformly in container, standby;
B, according to aqueous phase recipe requirements, each raw material is added in a tool stirring, condensing tube and charge door there-necked flask;By system temperature Rise to 33 DEG C, start stirring until each component is sufficiently mixed dissolving;
C, oil mixture step A prepared are poured in the aqueous phase there-necked flask that step B prepares;Keep reactor stirs Speed be 210 revs/min, make oil phase form uniform bead and be dispersed in the aqueous phase prepared in advance;It is warming up to 73 DEG C, directly Shape to bead;
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 2.25 hours;Polymerization reaction system is warming up to 85 DEG C, insulation 2.75 individual hour;Polymerization reaction system is warming up to 90 DEG C, is incubated 2.8 hours;Reaction system is cooled to 42 DEG C, leaches tree Fat bead;
E, employing ethanol carry out drip washing to resin, and the impurity of removing resin air-dries and i.e. obtains polyacrylic resin.

Claims (2)

1. an acrylic resin, it is characterised in that: include following raw materials by weight:
Oil phase:
Methyl methacrylate 30-40 part
Acrylonitrile 5-10 part
Lauryl acrylate 3-5 part
Butyl acrylate 5-10 part
Azodiisobutyronitrile 1-3 part
Aqueous phase:
Polyvinyl alcohol 3-5 part
Gelatin 5-10 part
NaCl 10-20 part
CaCO35 parts
Deionized water 500 parts.
The preparation method of a kind of acrylic resin the most according to claim 1, it is characterised in that: include that following technique walks Rapid:
A, accurately weigh each raw material in oil phase according to recipe requirements and be sufficiently mixed uniformly in container, standby;
B, according to aqueous phase recipe requirements, each raw material is added in a tool stirring, condensing tube and charge door there-necked flask;By system temperature Rise to 30-50 DEG C, start stirring until each component is sufficiently mixed dissolving;
C, oil mixture step A prepared are poured in the aqueous phase there-necked flask that step B prepares;Keep reactor stirs Speed be 200-300 rev/min, make oil phase form uniform bead and be dispersed in the aqueous phase prepared in advance;It is warming up to 72- 76 DEG C, until bead sizing;
D, polymerization reaction system temperature is raised to 80 DEG C, insulation 2-3 hour;Polymerization reaction system is warming up to 85 DEG C, insulation 2-3 hour;Polymerization reaction system is warming up to 90 DEG C, insulation 2-3 hour;Reaction system is cooled to 30-50 DEG C, leaches Resin bead;
E, employing ethanol carry out drip washing to resin, and the impurity of removing resin air-dries and i.e. obtains polyacrylic resin.
CN201610730897.2A 2016-08-26 2016-08-26 A kind of acrylic resin and preparation method thereof Pending CN106084119A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610730897.2A CN106084119A (en) 2016-08-26 2016-08-26 A kind of acrylic resin and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610730897.2A CN106084119A (en) 2016-08-26 2016-08-26 A kind of acrylic resin and preparation method thereof

Publications (1)

Publication Number Publication Date
CN106084119A true CN106084119A (en) 2016-11-09

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610730897.2A Pending CN106084119A (en) 2016-08-26 2016-08-26 A kind of acrylic resin and preparation method thereof

Country Status (1)

Country Link
CN (1) CN106084119A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106674414A (en) * 2017-01-19 2017-05-17 中蓝晨光化工研究设计院有限公司 Acrylic resin and preparation method thereof
CN108676114A (en) * 2018-05-08 2018-10-19 河南省科学院化学研究所有限公司 A kind of synthetic method of acrylic resin

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106674414A (en) * 2017-01-19 2017-05-17 中蓝晨光化工研究设计院有限公司 Acrylic resin and preparation method thereof
CN108676114A (en) * 2018-05-08 2018-10-19 河南省科学院化学研究所有限公司 A kind of synthetic method of acrylic resin

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Application publication date: 20161109