CN106916247A - PMMA performed polymers and its preparation method and application - Google Patents

PMMA performed polymers and its preparation method and application Download PDF

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Publication number
CN106916247A
CN106916247A CN201710192671.6A CN201710192671A CN106916247A CN 106916247 A CN106916247 A CN 106916247A CN 201710192671 A CN201710192671 A CN 201710192671A CN 106916247 A CN106916247 A CN 106916247A
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performed polymers
pmma
pmma performed
preparation
initiator
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CN106916247B (en
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杜振勇
郝迎军
胡丽梅
何阳
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Beijing Huateng Dongguang Technology Development Co Ltd
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Beijing Huateng Dongguang Technology Development Co Ltd
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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
    • 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
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • 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
    • C09D133/08Homopolymers or copolymers of acrylic acid esters
    • 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
    • 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
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate

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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)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Sealing Material Composition (AREA)
  • Polymerisation Methods In General (AREA)

Abstract

The invention discloses a kind of PMMA performed polymers and its preparation method and application, belong to materials synthesis field.Above-mentioned PMMA performed polymers are prepared from by the component of following weight portion:130 180 parts of methyl methacrylate, 150 200 parts of diluent, 0.05 0.2 parts of initiator, 0.1 0.8 parts of paraffin, 0.1 0.8 parts of Tertiary amine accelerators.The invention provides a kind of PMMA performed polymers and its preparation method and application, wherein, the PMMA performed polymers material of preparation can stable storage more than 1 year under the conditions of normal temperature lucifuge, and constructed in 35~35 DEG C of temperature ranges, firm time is short, excellent performance, can be used for polymer concrete, the packing material of concrete structure seam, bridge waterproof, colored road surface, the field such as mattess that has anticorrosion requirement.

Description

PMMA performed polymers and its preparation method and application
Technical field
The present invention relates to a kind of performed polymer materials synthesis field, more particularly to a kind of PMMA performed polymers and preparation method thereof and Using.
Background technology
At present, the production of domestic polymetylmethacrylate performed polymer is mainly used in lucite and (is commonly called as acrylic Plate) production, the production process of acrylic board is divided into two steps, and PMMA performed polymers are synthesized first, and performed polymer exists again then Mix and be poured into predetermined mould, final molding with follow-up initiator in the time of regulation.If do not poured in time Operation is built, PMMA performed polymers cause damage there is autohemagglutination.Simultaneously as PMMA performed polymers are mainly used in the life of acrylic board Produce, therefore, the composition of raw materials of product is substantially stationary, and properties of product cannot change.
PMMA performed polymers be exactly with monomers such as MMA, BA, 2-EHA as primary raw material, by radical reaction, react into During capable position suitable to stage casing, using polymerization inhibitor and end-capping reagent, in the state of storage life activity, obtained after terminating reaction Polymer (or prepolymer).In the subsequent construction stage, reactivated by the method for adding peroxide unfinished Late phase reaction, can fast reaction, and eventually become high performance material.But existing acrylic board PMMA pre-polymerization body techniques The PMMA performed polymers single, property of formula of middle preparation is substantially stationary, and storage time is short, it is impossible to meet engineering material change of properties Requirement that is many, needing post coat.
The content of the invention
For PMMA performed polymer material characters are single, Storage period is short, normal temperature in the existing acrylic board pre-polymerization body technique of solution The problems such as particularly low temperature is not susceptible to polymerisation, the present invention provides a kind of PMMA performed polymers and its preparation method and application.
In order to solve the above technical problems, present invention offer technical scheme is as follows:
On the one hand, the present invention provides a kind of PMMA performed polymers, is prepared from by the component of following weight portion:
Preferably, above-mentioned PMMA performed polymers, are prepared from by the component of following weight portion:
Preferably, above-mentioned PMMA performed polymers, are prepared from by the component of following weight portion:
Further, the diluent is the one kind or many in methacrylic acid, butyl acrylate or Isooctyl acrylate monomer Kind;Crosslinking can be played, system viscosity is reduced, is improved the effect such as curing rate.
The initiator is azodiisobutyronitrile.
On the other hand, the present invention also provides a kind of preparation method of above-mentioned PMMA performed polymers, including:
Step 1:25-35% methyl methacrylates, 85-90% diluents, stirring mixing are sequentially added in reactor Uniformly;
Step 2:Remaining methyl methacrylate, remaining diluent, initiator are sequentially added in monomer dropping tank, It is uniformly mixed;
Step 3:Material in reactor is heated up and is controlled at 95-105 DEG C, under stirring, by monomer dropping tank Monomer gob be added in reactor;
Step 4:After being added dropwise to complete, isothermal holding is carried out to reactor material;
Step 5:To paraffin, Tertiary amine accelerators are added in step 4, it is well mixed, analyzes qualified rear packaging.
Further, the monomer dropping time is 4-6 hours in the step 3.
Further, isothermal holding is under stirring, to keep temperature of charge 1 hour in kettle in the step 4.
Another further aspect, the present invention also provides a kind of application of above-mentioned PMMA performed polymers, and the PMMA performed polymers add when using Plus rear initiator.
Further, the rear initiator is benzoyl peroxide, and the addition of the rear initiator is PMMA performed polymers 0.2-0.4wt%.
Further, the PMMA performed polymers can be used for polymer concrete, packing material, the bridge of concrete structure seam Waterproof, colored road surface, the mattess field for having anticorrosion requirement.
The invention provides a kind of PMMA performed polymers and its preparation method and application, have the advantages that:
1) the PMMA performed polymers material for preparing can stable storage more than 1 year under the conditions of normal temperature lucifuge;
2) the PMMA performed polymers material for preparing is in -30-35 DEG C of scope energy excellent performance;
3) it is short to the initiator after-hardening time after being added in PMMA performed polymers, and can be right according to the use requirement of client The adding proportion of various monomers is adjusted, and realizes that final polymer has from firmly to soft mode of appearance and correspondence characteristic, can For polymer concrete, packing material, bridge waterproof, colored road surface, the coagulation that has anticorrosion requirement of concrete structure seam Soil Mian Deng fields.
Specific embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with specific implementation Example is described in detail.
Such scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are for illustrating The present invention and be not limited to limit the scope of the present invention.The implementation condition used in embodiment can be done according to the situation of specific product Further adjustment, unreceipted implementation condition is usually the condition in normal experiment.
Material used, reagent etc., commercially obtain in following embodiments.
The present invention provides a kind of PMMA performed polymers and its preparation method and application, and detailed process is referring to following embodiments.
Embodiment 1
A kind of PMMA performed polymers, are prepared from by the component of following weight portion:
The preparation method of above-mentioned PMMA performed polymers, including:
Step 1:32.5 parts of methyl methacrylates, 127.5 parts of diluents are sequentially added in reactor, stirring mixing is equal It is even;
Step 2:Remaining methyl methacrylate, remaining diluent, initiator are sequentially added in monomer dropping tank, It is uniformly mixed;
Step 3:Material in reactor is heated up and is controlled at 95 DEG C, under stirring, by the list in monomer dropping tank To in reactor, the monomer dropping time is 4 hours to body material dropping, and reaction temperature is 95 DEG C;
Step 4:After being added dropwise to complete, isothermal holding is carried out to reactor material:Under stirring, material temperature in kettle is kept Degree 1 hour;
Step 5:To paraffin, Tertiary amine accelerators are added in step 4, it is well mixed, analyzes qualified rear packaging.
Embodiment 2
A kind of PMMA performed polymers, are prepared from by the component of following weight portion:
The preparation method of above-mentioned PMMA performed polymers, including:
Step 1:25% methyl methacrylate, 85% diluent is sequentially added in reactor, stirring mixing is equal It is even;
Step 2:Remaining methyl methacrylate, remaining diluent, initiator are sequentially added in monomer dropping tank, It is uniformly mixed;
Step 3:Material in reactor is heated up and is controlled at 100 DEG C, under stirring, by the list in monomer dropping tank To in reactor, the monomer dropping time is 5 hours to body material dropping;
Step 4:After being added dropwise to complete, isothermal holding is carried out to reactor material:Under stirring, material temperature in kettle is kept Degree 1 hour;
Step 5:To paraffin, Tertiary amine accelerators are added in step 4, it is well mixed, analyzes qualified rear packaging.
Embodiment 3
A kind of PMMA performed polymers, are prepared from by the component of following weight portion:
The preparation method of above-mentioned PMMA performed polymers, including:
Step 1:35% methyl methacrylate, 90% diluent is sequentially added in reactor, stirring mixing is equal It is even;
Step 2:Remaining methyl methacrylate, remaining diluent, initiator are sequentially added in monomer dropping tank, It is uniformly mixed;
Step 3:Material in reactor is heated up and is controlled at 105 DEG C, under stirring, by the list in monomer dropping tank To in reactor, the monomer dropping time is 4 hours to body material dropping;
Step 4:After being added dropwise to complete, isothermal holding is carried out to reactor material:Under stirring, material temperature in kettle is kept Degree 1 hour;
Step 5:To paraffin, Tertiary amine accelerators are added in step 4, it is well mixed, analyzes qualified rear packaging.
Embodiment 4
A kind of PMMA performed polymers, are prepared from by the component of following weight portion:
The preparation method of above-mentioned PMMA performed polymers, including:
Step 1:30% methyl methacrylate, 90% diluent is sequentially added in reactor, stirring mixing is equal It is even;
Step 2:Remaining methyl methacrylate, remaining diluent, initiator are sequentially added in monomer dropping tank, It is uniformly mixed;
Step 3:Material in reactor is heated up and is controlled at 95 DEG C, under stirring, by the list in monomer dropping tank To in reactor, the monomer dropping time is 6 hours to body material dropping;
Step 4:After being added dropwise to complete, isothermal holding is carried out to reactor material:Under stirring, material temperature in kettle is kept Degree 1 hour;
Step 5:To paraffin, Tertiary amine accelerators are added in step 4, it is well mixed, analyzes qualified rear packaging.
Embodiment 5
A kind of PMMA performed polymers, are prepared from by the component of following weight portion:
The preparation method of above-mentioned PMMA performed polymers, including:
Step 1:25% methyl methacrylate, 85% diluent is sequentially added in reactor, stirring mixing is equal It is even;
Step 2:Remaining methyl methacrylate, remaining diluent, initiator are sequentially added in monomer dropping tank, It is uniformly mixed;
Step 3:Material in reactor is heated up and is controlled at 105 DEG C, under stirring, by the list in monomer dropping tank To in reactor, the monomer dropping time is 5 hours to body material dropping;
Step 4:After being added dropwise to complete, isothermal holding is carried out to reactor material:Under stirring, material temperature in kettle is kept Degree 1 hour;
Step 5:To paraffin, Tertiary amine accelerators are added in step 4, it is well mixed, analyzes qualified rear packaging.
Performance detection is carried out to PMMA performed polymers prepared by above-described embodiment, 1 is the results are shown in Table.
Table 1
As shown in Table 1, under the conditions of the PMMA performed polymer normal temperature lucifuges that prepared by the present invention can stable storage more than 1 year, wherein PMMA performed polymers content is 35%-45%, and MMA contents reach 40%-90%, and viscosity is also from 1500MPas to 4500MPa S, each monomer of ratio can be according to the actual requirements to to(for) the performance of PMMA performed polymers is adjusted.
The present invention also provides a kind of application of above-mentioned PMMA performed polymers, and the PMMA performed polymers of preparation can be applied to polymer and mix Solidifying soil, the packing material of concrete structure seam, bridge waterproof, colored road surface, the mattess field that has anticorrosion requirement. PMMA performed polymers to be added when using after initiator, the addition of rear initiator is the 0.2-0.4wt% of PMMA performed polymers ,- Its firm time is surveyed in the range of 35~35 DEG C and is shown in Table 2.
Table 2
As shown in Table 2, by initiator after addition, may be such that PMMA performed polymers are quick in -35~35 DEG C of temperature ranges Polymerization, firm time is 25~90min, and firm time is short.
In summary, the invention provides a kind of PMMA performed polymers and its preparation method and application, wherein, the PMMA of preparation Performed polymer material can stable storage more than 1 year, and, property short in -35~35 DEG C of scope energy firm times under the conditions of normal temperature lucifuge Can it is excellent, can be used for polymer concrete, concrete structure seam packing material, bridge waterproof, colored road surface, have anticorrosion will The fields such as the mattess asked.
Experiment provided above is only preferably example of the invention, the protection domain being not intended to limit the present invention.Should When pointing out, for those skilled in the art, on the premise of principle of the present invention is not departed from, can be with Some improvements and modifications are made, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (10)

1. a kind of PMMA performed polymers, it is characterised in that be prepared from by the component of following weight portion:
2. PMMA performed polymers according to claim 1, it is characterised in that be prepared from by the component of following weight portion:
3. PMMA performed polymers according to claim 2, it is characterised in that be prepared from by the component of following weight portion:
4. according to any described PMMA performed polymers of claim 1-3, it is characterised in that the diluent be methacrylic acid, One or more in butyl acrylate or Isooctyl acrylate monomer;
The initiator is azodiisobutyronitrile.
5. the preparation method of any described PMMA performed polymers of claim 1-4, it is characterised in that including:
Step 1:25-35%, the 85-90% of diluent of methyl methacrylate, stirring mixing are sequentially added in reactor Uniformly;
Step 2:Remaining methyl methacrylate, remaining diluent, initiator are sequentially added in monomer dropping tank, is stirred It is well mixed;
Step 3:Material in reactor is heated up and is controlled at 95-105 DEG C, under stirring, by the list in monomer dropping tank Body material dropping is in reactor;
Step 4:After being added dropwise to complete, isothermal holding is carried out to reactor material;
Step 5:To adding paraffin, Tertiary amine accelerators to be well mixed in step 4, qualified rear packaging is analyzed.
6. the preparation method of PMMA performed polymers according to claim 5, it is characterised in that monomer dropping in the step 3 Time is 4-6 hours.
7. the preparation method of PMMA performed polymers according to claim 5, it is characterised in that isothermal holding in the step 4 It is under stirring, to keep temperature of charge 1 hour in kettle.
8. the application of any described PMMA performed polymers of claim 1-4, it is characterised in that the PMMA performed polymers add when using Plus rear initiator.
9. the application of PMMA performed polymers according to claim 8, it is characterised in that the rear initiator is benzoyl peroxide first Acyl;The addition of the rear initiator is the 0.2-0.4wt% of PMMA performed polymers.
10. the application of PMMA performed polymers according to claim 8, it is characterised in that for polymer concrete, concrete The packing material of structural joint, bridge waterproof, colored road surface, the mattess field that has anticorrosion requirement.
CN201710192671.6A 2017-03-28 2017-03-28 PMMA performed polymer and its preparation method and application Active CN106916247B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108373519A (en) * 2017-12-28 2018-08-07 西安工业大学 Solvent-free quick-dry type super-high solid content methyl methacrylate coating resin and its synthetic method
CN115322606A (en) * 2022-08-30 2022-11-11 四川鑫环球科技有限公司 MMA (methyl methacrylate) road surface antiskid coating and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1107752A (en) * 1977-10-06 1981-08-25 Masahiro Yuyama Process for continuous production of prepolymer syrups
JP2002234921A (en) * 2001-02-13 2002-08-23 Mitsubishi Rayon Co Ltd Odor-less acrylic syrup composition

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1107752A (en) * 1977-10-06 1981-08-25 Masahiro Yuyama Process for continuous production of prepolymer syrups
JP2002234921A (en) * 2001-02-13 2002-08-23 Mitsubishi Rayon Co Ltd Odor-less acrylic syrup composition

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108373519A (en) * 2017-12-28 2018-08-07 西安工业大学 Solvent-free quick-dry type super-high solid content methyl methacrylate coating resin and its synthetic method
CN108373519B (en) * 2017-12-28 2020-07-28 西安工业大学 Solvent-free quick-drying type ultrahigh-solid-content methyl methacrylate coating resin and synthesis method thereof
CN115322606A (en) * 2022-08-30 2022-11-11 四川鑫环球科技有限公司 MMA (methyl methacrylate) road surface antiskid coating and preparation method thereof

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