CN107236076A - The preparation method of the impact-resistant acrylic resin of high rigidity - Google Patents

The preparation method of the impact-resistant acrylic resin of high rigidity Download PDF

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Publication number
CN107236076A
CN107236076A CN201710580302.4A CN201710580302A CN107236076A CN 107236076 A CN107236076 A CN 107236076A CN 201710580302 A CN201710580302 A CN 201710580302A CN 107236076 A CN107236076 A CN 107236076A
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CN
China
Prior art keywords
acrylic resin
impact
weight
high rigidity
percentage
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710580302.4A
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Chinese (zh)
Inventor
薛正彪
惠正权
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Sanmu Chemical Co Ltd
Jiangsu Sanmu Group Corp
Original Assignee
Jiangsu Sanmu Chemical Co Ltd
Jiangsu Sanmu Group Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Sanmu Chemical Co Ltd, Jiangsu Sanmu Group Corp filed Critical Jiangsu Sanmu Chemical Co Ltd
Priority to CN201710580302.4A priority Critical patent/CN107236076A/en
Publication of CN107236076A publication Critical patent/CN107236076A/en
Pending legal-status Critical Current

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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
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00Coating compositions 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04Homopolymers or copolymers of esters
    • C09D133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/10Homopolymers or copolymers of methacrylic acid esters
    • C09D133/12Homopolymers or copolymers of methyl methacrylate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Graft Or Block Polymers (AREA)
  • Laminated Bodies (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention discloses impact-resistant acrylic resin of a kind of high rigidity and preparation method thereof, it is made up of the raw material of following weight percents:Methyl methacrylate 30% 35%, hy-droxybutyl 7.4% 10%, butyl acrylate 2.5% 5%, acrylic acid 1 2%, initiator 2% 3%, organic solvent 30% 50%.The present invention is made up of and optimal synthesis technique many experiments preferred feedstock, and the acrylic resin paint prepared has excellent adhesive force, and glossiness is good, and with excellent hardness and impact resistance, achieves extraordinary technique effect.

Description

The preparation method of the impact-resistant acrylic resin of high rigidity
Technical field
The present invention relates to a kind of coating, and in particular to a kind of impact-resistant acrylic resin of environmentally friendly high rigidity and its preparation Method, belongs to technical field of polymer materials.
Background technology
Impact property is a kind of traditional performance of coating, mainly in car paint, and ratio is required in terms of engineering machinery coating It is higher, it will necessarily reduce the hardness of coating while conventional thermosetting acrylic resin improves impact property at present.From structure From the point of view of coating impact property with resins synthesis when the long Isooctyl acrylate monomer of the ester chain that uses it is relevant, the present invention is adopted With hy-droxybutyl so that the impact property that resin can still have under higher hardness.
The content of the invention
Goal of the invention:The purpose of the present invention is that in view of the shortcomings of the prior art, by many experiments, there is provided a kind of high rigidity Excellent acrylic resin of impact property and preparation method thereof.
Technical scheme, to realize object above, the technical solution adopted by the present invention is:
A kind of impact-resistant acrylic resin of high rigidity, it is made up of the raw material of following weight percents:
Methyl methacrylate 30%-35%, hy-droxybutyl 7.4%-10%, butyl acrylate 2.5%-5%, third Olefin(e) acid 1-2%, initiator 2%-3%, organic solvent 30%-50%.
A kind of preparation method of the impact-resistant acrylic resin of high rigidity, it comprises the following steps:
(1) initiator of methyl methacrylate, butyl acrylate, hy-droxybutyl, acrylic acid, 90% deal is mixed Close uniform, obtain mix monomer;
(2) organic solvent is put into reactor, is heated to reflux state;
(3) monomer that step (1) is well mixed is put into dropping tank, and mix monomer is added dropwise, and time for adding is that 2.5-3 is small When;2 hours are kept at reflux;Insulation finishes the initiator for adding remaining 10% deal;It is incubated 2 two hours;
(4) reaction is cooled to 100 DEG C after terminating, and filtering obtains acrylic resin.
Preferably, the preparation method of the impact-resistant acrylic resin of above-described high rigidity, methacrylic acid The percentage by weight of methyl esters is that 30%-35%, the percentage by weight of hy-droxybutyl are 7.4%-10%, butyl acrylate Percentage by weight be 2.5%-5%, the percentage by weight of acrylic acid be 1-2%, the percentage by weight of initiator be 2%-3%, The percentage by weight of organic solvent is 30%-50%.
Preferably, the preparation method of the impact-resistant acrylic resin of above-described high rigidity, organic solvent is Dimethylbenzene;Initiator is TBPB (peroxidized t-butyl perbenzoate).
The present invention is screened by many experiments, and the cross-linking monomer commonly used in acrylic resin is hydroxy-ethyl acrylate and propylene Sour hydroxypropyl acrylate, the acrylic resin impact synthesized using these carboxylic monomers will reach that 50Kg.cm hardness of paint films need to be reduced to Once, the present invention passes through the resin of Select to use hy-droxybutyl synthesis to 1H, and in the case where hardness reaches 2H, impact is appointed 50Kg.cm can so be reached.
Beneficial effect:Compared to the prior art, the present invention has the following advantages:
The present invention obtains optimal raw material by many experiments screening and constitutes and match, and is preferably gone out by many experiments optimal Synthesis technique.Whole preparation technology is reasonable in design, and the acrylic resin prepared has excellent hardness and impact resistance Energy.
Embodiment
Embodiment 1
1st, the preparation method of the impact-resistant acrylic resin of a kind of high rigidity, it comprises the following steps:
(1) by 42 grams of methyl methacrylate, 6 grams of butyl acrylate, 8 grams of hy-droxybutyl, 1.5 grams of acrylic acid, 2.25 grams of TBPB (the 90% of total amount) is uniformly mixed, and obtains mix monomer;
(2) by 40 grams of input reactors of dimethylbenzene, it is heated to reflux state;
(3) monomer that step (1) is well mixed was put into dropping tank, with 2.5-3 hours uniform dropwise addition mix monomers;It is added dropwise Finish, 2 hours of reaction are kept at reflux;Insulation is finished;Add remaining 0.25 gram of initiator (the 10% of total amount);After Reacted 2 hours under continuous reflux state, cool to 100 degree, obtain acrylic resin.
2nd, performance test is carried out to obtained high acrylic resin paint made above, test result is as shown in table 1 below:
Table 1 can testing result
Film thickness (μ) 24
Adhesive force 1 grade
Gloss 90
Hardness 2H
Impact resistance (Kg.cm) 50
More than test result indicates that, the acrylic resin paint for preparing of the present invention has excellent adhesive force, light Damp degree and excellent hardness and impact resistance, achieve extraordinary technological progress.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (4)

1. a kind of impact-resistant acrylic resin of high rigidity, it is characterised in that it is made up of the raw material of following weight percents:
Methyl methacrylate 30%-35%, hy-droxybutyl 7.4%-10%, butyl acrylate 2.5%-5%, acrylic acid 1-2%, initiator 2%-3%, organic solvent 30%-50%.
2. a kind of preparation method of the impact-resistant acrylic resin of high rigidity, it is characterised in that it comprises the following steps:
(1) initiator of methyl methacrylate, butyl acrylate, hy-droxybutyl, acrylic acid, 90% deal is mixed equal It is even, obtain mix monomer;
(2) organic solvent is put into reactor, is heated to reflux state;
(3) monomer that step (1) is well mixed is put into dropping tank, and mix monomer is added dropwise, and time for adding is 2.5-3 hours; 2 hours are kept under reflux state;Insulation finishes the initiator for adding remaining 10% deal;It is incubated 2 two hours;
(4) reaction is cooled to 100 DEG C after terminating, and filtering obtains acrylic resin.
3. the preparation method of the impact-resistant acrylic resin of high rigidity according to claim 2, it is characterised in that methyl-prop The percentage by weight of e pioic acid methyl ester is that 30%-35%, the percentage by weight of hy-droxybutyl are 7.4%-10%, acrylic acid fourth The percentage by weight of ester is that 2.5%-5%, the percentage by weight of acrylic acid are that 1-2%, the percentage by weight of initiator are 2%- 3%th, the percentage by weight of organic solvent is 30%-50%.
4. the preparation method of the impact-resistant acrylic resin of high rigidity according to claim 3, it is characterised in that You Jirong Agent is dimethylbenzene;Initiator is peroxidized t-butyl perbenzoate.
CN201710580302.4A 2017-07-17 2017-07-17 The preparation method of the impact-resistant acrylic resin of high rigidity Pending CN107236076A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710580302.4A CN107236076A (en) 2017-07-17 2017-07-17 The preparation method of the impact-resistant acrylic resin of high rigidity

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710580302.4A CN107236076A (en) 2017-07-17 2017-07-17 The preparation method of the impact-resistant acrylic resin of high rigidity

Publications (1)

Publication Number Publication Date
CN107236076A true CN107236076A (en) 2017-10-10

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CN (1) CN107236076A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109053947A (en) * 2018-07-17 2018-12-21 万华化学集团股份有限公司 A kind of thermosetting acrylic resin and its preparation method and use having both high rigidity and resistance to deep-draw
CN109438605A (en) * 2018-09-17 2019-03-08 万华化学集团股份有限公司 Water-soluble and aqueous dispersion type Hydroxylated acrylic resin and its preparation method and application
CN110804124A (en) * 2019-11-06 2020-02-18 广昌立骅科技股份有限公司 High-hardness and high-toughness acrylic resin and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101407568A (en) * 2008-11-21 2009-04-15 山东轻工业学院 High solid low viscosity acrylic resin and preparation thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101407568A (en) * 2008-11-21 2009-04-15 山东轻工业学院 High solid low viscosity acrylic resin and preparation thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
化工部科技情报研究所: "《全国化工新产品应用手册》", 31 December 1992, 化工部科技情报研究所 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109053947A (en) * 2018-07-17 2018-12-21 万华化学集团股份有限公司 A kind of thermosetting acrylic resin and its preparation method and use having both high rigidity and resistance to deep-draw
CN109438605A (en) * 2018-09-17 2019-03-08 万华化学集团股份有限公司 Water-soluble and aqueous dispersion type Hydroxylated acrylic resin and its preparation method and application
CN109438605B (en) * 2018-09-17 2021-07-23 万华化学集团股份有限公司 Water-soluble and water-dispersible hydroxy acrylic resin and preparation method and application thereof
CN110804124A (en) * 2019-11-06 2020-02-18 广昌立骅科技股份有限公司 High-hardness and high-toughness acrylic resin and preparation method thereof

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Application publication date: 20171010