CN106380537B - The method that reaction under high pressure produces high-solid lower-viscosity acrylic resin - Google Patents

The method that reaction under high pressure produces high-solid lower-viscosity acrylic resin Download PDF

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CN106380537B
CN106380537B CN201610890807.6A CN201610890807A CN106380537B CN 106380537 B CN106380537 B CN 106380537B CN 201610890807 A CN201610890807 A CN 201610890807A CN 106380537 B CN106380537 B CN 106380537B
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acrylic resin
propylene glycol
monomethyl ether
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CN106380537A (en
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张丹军
徐俊
杨剑挺
张辉
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SUZHOU JIAXIANG RESIN CO Ltd
Taixing Best Resin Co Ltd
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SUZHOU JIAXIANG RESIN CO Ltd
Taixing Best Resin 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
    • C08F212/00Copolymers 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 an aromatic carbocyclic ring
    • C08F212/02Monomers containing only one unsaturated aliphatic radical
    • C08F212/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06Hydrocarbons
    • C08F212/08Styrene
    • 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
    • C09D125/00Coating 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 an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
    • C09D125/02Homopolymers or copolymers of hydrocarbons
    • C09D125/04Homopolymers or copolymers of styrene
    • C09D125/08Copolymers of styrene
    • C09D125/14Copolymers of styrene with unsaturated 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

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

Abstract

The present invention relates to a kind of methods of reaction under high pressure production high-solid lower-viscosity acrylic resin, belong to the technical field of coating.The method of the reaction under high pressure production high-solid lower-viscosity acrylic resin of the present invention, includes the following steps:Solvent xylene and propylene glycol monomethyl ether are added in reaction kettle, stirred evenly;Mix monomer and initiator are added in reaction kettle, stirred evenly;Closed reactor, logical non-reactive gas are forced into 0.6~1.0MPa, and are warming up to 175~185 DEG C, insulation reaction 1.0~3.0 hours, are cooled to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can.Resin formulations prepared by method using the present invention are into after coating, and gloss, chemical resistance, the application property of coating are also greatly improved, suitable for industrial circles such as automobile, machine components.

Description

The method that reaction under high pressure produces high-solid lower-viscosity acrylic resin
Technical field
The present invention relates to the technical field of coating, specifically, the present invention relates to a kind of reaction under high pressures to produce high-solid lower-viscosity The method of acrylic resin.
Background technology
With global energy-saving and environmental protection realize enhancing, high solid, low VOC emission coating becoming mainstream.And make For film forming matter main inside coating:Acrylic resin needs the requirement for reaching high-solid lower-viscosity.However acrylic acid traditional at present The production technology of resin is produced for non-pressure process, it is difficult to produce high-solid lower-viscosity, acrylic resin of fine qualities.Existing normal pressure Method technique is as follows:25% solvent xylene, propylene glycol monomethyl ether etc. are put into reaction kettle bottom, are warming up to reflux temperature 135 ± 2 DEG C, then 75% mix monomer is slowly added dropwise:Methyl methacrylate (first methyl esters), butyl acrylate, styrene etc. and initiator: Cumyl peroxide etc. keeps the temperature 4 hours, until reaction terminates.The shortcoming of the technique has:Temperature restriction is produced in solvent Boiling point, the boiling point of Conventional solvents is relatively low, and range is at 80~136 DEG C.However the decomposition temperature of initiator is higher, range is 140 ~160 DEG C.So causing when producing high-solid lower-viscosity acrylic resin, decomposition of initiator speed is slow, and molecular resin amount is big, viscosity Height, molecular weight distribution are uneven.And in order to improve the distribution situation of molecular weight, if excessive uses molecular weight regulator for example Lauryl mercaptan etc., then the weatherability and chemical resistance that can lead to resin again decline, so as to influence the performance of coating.
Invention content
In order to solve above-mentioned technical problem of the prior art, the purpose of the present invention is to provide a kind of productions of reaction under high pressure The method of high-solid lower-viscosity acrylic resin.
In order to achieve the above-mentioned object of the invention, the first aspect of the present invention employs following technical scheme:
A kind of method of reaction under high pressure technique productions high-solid lower-viscosity acrylic resin, it is characterised in that include the following steps:
(1) solvent xylene and propylene glycol monomethyl ether are added in reaction kettle, stirred evenly;
(2) mix monomer and initiator are added in reaction kettle, stirred evenly;
(3) closed reactor, logical non-reactive gas are forced into 0.6~1.0MPa, and are warming up to 175~185 DEG C, heat preservation Reaction 1.0~3.0 hours is cooled to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can.
Wherein, the non-reactive gas is selected from nitrogen, inert gas or their mixed gas.
Wherein, the methyl methacrylate of the mix monomer including 25~35 parts by weight, 20~35 parts by weight benzene second The butyl acrylate of alkene and 10~20 parts by weight.
Wherein, the initiator is selected from cumyl peroxide, isopropyl benzene hydroperoxide, tert-butyl hydroperoxide or peroxide Change one kind in methyl ethyl ketone.
Wherein, the content of the initiator is 1.0~3.0 parts by weight.
Wherein, the parts by weight of the dimethylbenzene are 15~20 parts by weight, and the parts by weight of propylene glycol monomethyl ether are 8~12 weights Part is measured, and the weight ratio of the dimethylbenzene and propylene glycol monomethyl ether is 1.5~2:1.
Preferably, the mix monomer is by the methyl methacrylates of 25~35 parts by weight, 20~35 parts by weight The styrene and butyl acrylate of 10~20 parts by weight, the emulsion stability of 1.5~5.0 parts by weight and 2.0~3.5 parts by weight Hydrosulphonyl functionalized siloxanes composition.
Wherein, the hydrosulphonyl functionalized siloxanes is selected from 3- Mercaptopropyltriethoxysilanes, 3- mercaptopropyi front threes One kind in oxysilane, 3- mercaptopropyis methyl dimethoxysilane and 3- mercaptopropyi methyldiethoxysilanes.
Wherein, the emulsion stability is selected from acrylate, acrylic acid-N- propylcarbamics ethyl ester, (methyl) third One kind in olefin(e) acid-N- ethylaminos propyl ester and (methyl) acrylic acid-N- phenyl amino ethyl esters.
Compared with prior art, the method for reaction under high pressure technique productions high-solid lower-viscosity acrylic resin of the invention have with Lower advantageous effect:
The production that the method for reaction under high pressure technique productions high-solid lower-viscosity acrylic resin of the present invention is prepared with non-pressure process Condition ratio can reduce viscosity about 50%~100%, and ageing-resistant performance improves 30%~100% compared with non-pressure process; After the resin formulations coating of high-pressure process production, gloss, chemical resistance, the application property of coating are also greatly improved.Cause This, the acrylic resin of high-pressure process technique productions more meets the standard of current high-solid lower-viscosity coating.
Specific embodiment
Below with reference to specific embodiment to the side of reaction under high pressure of the present invention production high-solid lower-viscosity acrylic resin Method is further elaborated, more complete, accurate those skilled in the art to be helped to have inventive concept of the invention, technical solution True and deep understanding.
Embodiment 1
The acrylic resin of the present embodiment, raw material contain following parts by weight:The dimethylbenzene of 15 parts by weight, 10 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 25 parts by weight, the styrene of 20 parts by weight, 15 parts by weight butyl acrylate, 2.0 The cumyl peroxide of parts by weight.The preparation method of the acrylic resin, includes the following steps:First, by solvent diformazan Benzene and propylene glycol monomethyl ether are added in reaction kettle, are stirred evenly;Then, by methyl methacrylate, styrene, butyl acrylate and Cumyl peroxide is added in reaction kettle, is stirred evenly;Closed reactor leads to N20.6MPa is forced into, and is warming up to 175 DEG C, insulation reaction 2.0 hours is cooled to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can obtain the acrylic resin of high-solid lower-viscosity.
Embodiment 2
The acrylic resin of the present embodiment, raw material contain following parts by weight:The dimethylbenzene of 20 parts by weight, 12 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 30 parts by weight, the styrene of 30 parts by weight, the butyl acrylate of 20 parts by weight, 2.5 The cumyl peroxide of parts by weight.The preparation method of the acrylic resin, includes the following steps:First, by solvent diformazan Benzene and propylene glycol monomethyl ether are added in reaction kettle, are stirred evenly;Then, by methyl methacrylate, styrene, butyl acrylate and Cumyl peroxide is added in reaction kettle, is stirred evenly;Closed reactor leads to N20.8MPa is forced into, and is warming up to 180 DEG C, insulation reaction 2.0 hours is cooled to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can obtain the acrylic resin of high-solid lower-viscosity.
Embodiment 3
The acrylic resin of the present embodiment, raw material contain following parts by weight:The dimethylbenzene of 18 parts by weight, 10 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 20 parts by weight, the styrene of 25 parts by weight, the butyl acrylate of 20 parts by weight, 2.0 The cumyl peroxide of parts by weight.The preparation method of the acrylic resin, includes the following steps:First, by solvent diformazan Benzene and propylene glycol monomethyl ether are added in reaction kettle, are stirred evenly;Then, by methyl methacrylate, styrene, butyl acrylate and Cumyl peroxide is added in reaction kettle, is stirred evenly;Closed reactor leads to N20.8MPa is forced into, and is warming up to 180 DEG C, insulation reaction 2.0 hours is cooled to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can obtain the acrylic resin of high-solid lower-viscosity.
Embodiment 4
The acrylic resin of the present embodiment, raw material contain following parts by weight:The dimethylbenzene of 15 parts by weight, 10 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 25 parts by weight, the styrene of 20 parts by weight, the butyl acrylate of 15 parts by weight, 2.5 The peroxidating two of the acrylate of parts by weight, the 3- Mercaptopropyltriethoxysilanes of 2.0 parts by weight, 2.0 parts by weight Isopropylbenzene.The preparation method of the acrylic resin, includes the following steps:First, solvent xylene and propylene glycol monomethyl ether are added Enter in reaction kettle, stir evenly;Then, by methyl methacrylate, styrene, butyl acrylate, acrylate, 3- Mercaptopropyltriethoxysilane and cumyl peroxide are added in reaction kettle, are stirred evenly;Closed reactor leads to N2Pressurization To 0.6MPa, and 175 DEG C are warming up to, insulation reaction 2.0 hours is cooled to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can obtain The acrylic resin of high-solid lower-viscosity.
Embodiment 5
The acrylic resin of the present embodiment, raw material contain following parts by weight:The dimethylbenzene of 15 parts by weight, 10 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 25 parts by weight, the styrene of 20 parts by weight, the butyl acrylate of 15 parts by weight, 2.5 Acrylic acid-N- propylcarbamics the ethyl ester of parts by weight, the 3-mercaptopropyi trimethoxy silane of 2.0 parts by weight, the mistake of 2.0 parts by weight Aoxidize diisopropylbenzene (DIPB).The preparation method of the acrylic resin, includes the following steps:First, by solvent xylene and propylene glycol Methyl ether is added in reaction kettle, is stirred evenly;Then, by methyl methacrylate, styrene, butyl acrylate, acrylic acid-N- third Base amino ethyl ester, 3-mercaptopropyi trimethoxy silane and cumyl peroxide are added in reaction kettle, are stirred evenly;It is closed anti- Kettle is answered, leads to N20.6MPa is forced into, and is warming up to 175 DEG C, insulation reaction 2.0 hours is cooled to 100 DEG C hereinafter, simultaneously pressure release is extremely Normal pressure, you can obtain the acrylic resin of high-solid lower-viscosity.
Embodiment 6
The acrylic resin of the present embodiment, raw material contain following parts by weight:The dimethylbenzene of 15 parts by weight, 10 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 25 parts by weight, the styrene of 20 parts by weight, the butyl acrylate of 15 parts by weight, 5.0 Acrylic acid-N- propylcarbamics the ethyl ester of parts by weight, 3- mercaptopropyis methyldiethoxysilane, 2.0 parts by weight of 2.5 parts by weight Cumyl peroxide.The preparation method of the acrylic resin, includes the following steps:First, by solvent xylene and third Glycol methyl ether is added in reaction kettle, is stirred evenly;Then, by methyl methacrylate, styrene, butyl acrylate, acrylic acid- N- propylcarbamics ethyl ester, 3- mercaptopropyis methyldiethoxysilane and cumyl peroxide are added in reaction kettle, and stirring is equal It is even;Closed reactor leads to N2Be forced into 0.6MPa, and be warming up to 175 DEG C, insulation reaction 2.0 hours, be cooled to 100 DEG C hereinafter, And pressure release is to normal pressure, you can obtains the acrylic resin of high-solid lower-viscosity.
Comparative example 1
The acrylic resin of this comparative example, raw material contain following parts by weight:The dimethylbenzene of 15 parts by weight, 10 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 25 parts by weight, the styrene of 20 parts by weight, the butyl acrylate of 15 parts by weight, 2.0 The 3- Mercaptopropyltriethoxysilanes of parts by weight, the cumyl peroxide of 2.0 parts by weight.The preparation of the acrylic resin Method includes the following steps:First, solvent xylene and propylene glycol monomethyl ether are added in reaction kettle, stirred evenly;Then, will Methyl methacrylate, styrene, butyl acrylate, 3- Mercaptopropyltriethoxysilanes and cumyl peroxide add in anti- It answers in kettle, stirs evenly;Closed reactor leads to N20.6MPa is forced into, and is warming up to 175 DEG C, insulation reaction 2.0 hours, drop Temperature is to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can obtains acrylic resin.
Comparative example 2
The acrylic resin of this comparative example, raw material contain following parts by weight:The dimethylbenzene of 15 parts by weight, 10 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 25 parts by weight, the styrene of 20 parts by weight, the butyl acrylate of 15 parts by weight, 2.5 The acrylate of parts by weight, the mercaptoethanol of 2.0 parts by weight, 2.0 parts by weight cumyl peroxide.The propylene The preparation method of acid resin, includes the following steps:First, solvent xylene and propylene glycol monomethyl ether are added in reaction kettle, stirring Uniformly;Then, by methyl methacrylate, styrene, butyl acrylate, acrylate, mercaptoethanol and peroxidating Diisopropylbenzene (DIPB) is added in reaction kettle, is stirred evenly;Closed reactor leads to N20.6MPa is forced into, and is warming up to 175 DEG C, is kept the temperature Reaction 2.0 hours is cooled to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can obtain acrylic resin.
Comparative example 3
The acrylic resin of this comparative example, raw material contain following parts by weight:The dimethylbenzene of 15 parts by weight, 10 parts by weight Propylene glycol monomethyl ether, the methyl methacrylate of 25 parts by weight, the styrene of 20 parts by weight, the butyl acrylate of 15 parts by weight, 2.5 The 3- TSL 8330s of parts by weight, the mercaptoethanol of 2.0 parts by weight, 2.0 parts by weight cumyl peroxide. The preparation method of the acrylic resin, includes the following steps:First, solvent xylene and propylene glycol monomethyl ether are added in into reaction kettle It is interior, it stirs evenly;Then, by methyl methacrylate, styrene, butyl acrylate, 3- TSL 8330s, mercapto Base ethyl alcohol and cumyl peroxide are added in reaction kettle, are stirred evenly;Closed reactor leads to N20.6MPa is forced into, and is risen Temperature is to 175 DEG C, insulation reaction 2.0 hours, is cooled to 100 DEG C hereinafter, simultaneously pressure release is to normal pressure, you can obtain acrylic resin.
The acrylic resin solid part being prepared using above-described embodiment and comparative example can reach 65~75wt%, And viscosity is 1500~3000mPas.
Coating property is tested
The car paint of consisting of is configured using the acrylic resin that above-described embodiment and comparative example obtain as base-material:
The acrylic resin (70%) of 65 parts by weight
23.5 parts by weight titanium dioxides (R-930)
The levelling agent BYK-358 of 0.2 parts by weight
The mixed solvent of 18.5 parts by weight.
The mixed solvent is made of toluene, dimethylbenzene, butyl acetate and glycol dimethyl ether.And toluene:Dimethylbenzene: Butyl acetate:The molar ratio of glycol dimethyl ether is 2:4:3:1.
Coating property is as shown in Table 1 and Table 2:
Table 1
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6
Film thickness (μm) ~20 μm ~20 μm ~20 μm ~20 μm ~20 μm ~20 μm
60 ° of gloss (%) 93~98 93~98 93~98 93~98 93~98 93~98
Flexibility (mm) 1 1 1 1 1 1
Adhesive force (cross-hatching) 0~1 0~1 0~1 0 0 0
Hardness (swing rod method) 0.61~0.66 0.61~0.66 0.61~0.66 0.61~0.66 0.61~0.66 0.61~0.66
Petrol-resistance (24 hours) It is non-discolouring It is non-discolouring It is non-discolouring It is non-discolouring It is non-discolouring It is non-discolouring
Acid resistance (5% sulfuric acid) (d) 7~8 7~8 7~8 10~12 10~12 10~12
Artificial accelerated aging (h) > 1500 > 1500 > 1500 > 2000 > 2000 > 2000
Wherein, the acid resistance refer to paint film generation blister, wrinkle, coming off, changing colour or loss of gloss (albedo is less than 50%) number of days being subjected to when phenomenon generates.When artificial accelerated aging refers to that paint film to loss of gloss (albedo is less than 50%) generates The hourage being subjected to.
Table 2
Project Comparative example 1 Comparative example 2 Comparative example 3
Film thickness (μm) ~20 μm ~20 μm ~20 μm
60 ° of gloss (%) 93~98 93~98 93~98
Flexibility (mm) 1 1 1
Adhesive force (cross-hatching) 0 1 0~1
Hardness (swing rod method) 0.61~0.66 0.61~0.66 0.61~0.66
Petrol-resistance (24 hours) It is non-discolouring It is non-discolouring It is non-discolouring
Acid resistance (5% sulfuric acid) (d) 7~8 7~8 7~8
Artificial accelerated aging (h) > 1500 > 1500 > 1500
Wherein, the acid resistance refer to paint film generation blister, wrinkle, coming off, changing colour or loss of gloss (albedo is less than 50%) number of days being subjected to when phenomenon generates.When artificial accelerated aging refers to that paint film to loss of gloss (albedo is less than 50%) generates The hourage being subjected to.
For the ordinary skill in the art, specific embodiment is only exemplarily described the present invention, Obviously the present invention specific implementation is not subject to the restrictions described above, as long as employ the inventive concept and technical scheme of the present invention into The improvement of capable various unsubstantialities or it is not improved by the present invention design and technical solution directly apply to other occasions , within protection scope of the present invention.

Claims (6)

  1. A kind of 1. method of reaction under high pressure technique productions high-solid lower-viscosity acrylic resin, it is characterised in that include the following steps:
    (1) solvent xylene and propylene glycol monomethyl ether are added in reaction kettle, stirred evenly;The parts by weight of the dimethylbenzene are 15 ~20 parts by weight, the parts by weight of propylene glycol monomethyl ether are 8~12 parts by weight, and the weight of the dimethylbenzene and propylene glycol monomethyl ether Than being 1.5~2:1;
    (2) mix monomer and initiator are added in reaction kettle, stirred evenly;The mix monomer by 25~35 parts by weight first Base methyl acrylate, the butyl acrylate of the styrene of 20~35 parts by weight and 10~20 parts by weight, 1.5~5.0 parts by weight The hydrosulphonyl functionalized siloxanes composition of emulsion stability and 2.0~3.5 parts by weight;
    (3) closed reactor, logical non-reactive gas are forced into 0.6~1.0MPa, and are warming up to 175~185 DEG C, insulation reaction 1.0~3.0 hours, 100 DEG C were cooled to hereinafter, simultaneously pressure release is to normal pressure, you can.
  2. 2. according to the method described in claim 1, it is characterized in that:The non-reactive gas be selected from nitrogen, inert gas or Their mixed gas.
  3. 3. according to the method described in claim 1, it is characterized in that:The initiator is selected from cumyl peroxide, isopropylbenzene One kind in hydrogen peroxide, tert-butyl hydroperoxide or methyl ethyl ketone peroxide.
  4. 4. according to the method described in claim 3, it is characterized in that:The content of the initiator is 1.0~3.0 parts by weight.
  5. 5. according to the method described in claim 1, it is characterized in that:The hydrosulphonyl functionalized siloxanes is selected from 3- mercaptopropyis Triethoxysilane, 3-mercaptopropyi trimethoxy silane, 3- mercaptopropyis methyl dimethoxysilane and 3- mercaptopropyi first One kind in base diethoxy silane.
  6. 6. according to the method described in claim 1, it is characterized in that:The emulsion stability is selected from acrylate, third Olefin(e) acid-N- propylcarbamics ethyl ester, (methyl) acrylic acid-N- ethylaminos propyl ester and (methyl) acrylic acid-N- phenyl amino ethyl esters In one kind.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101921357A (en) * 2010-08-17 2010-12-22 江门市制漆厂有限公司 High-solid low-viscosity hydroxy acrylic resin and preparation process thereof
CN103130946A (en) * 2013-03-27 2013-06-05 苏州双象光学材料有限公司 Continuous production process of polymethyl methacrylate
CN104031202A (en) * 2014-06-17 2014-09-10 中国科学院化学研究所 Polyacrylic acid printing ink resin and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101921357A (en) * 2010-08-17 2010-12-22 江门市制漆厂有限公司 High-solid low-viscosity hydroxy acrylic resin and preparation process thereof
CN103130946A (en) * 2013-03-27 2013-06-05 苏州双象光学材料有限公司 Continuous production process of polymethyl methacrylate
CN104031202A (en) * 2014-06-17 2014-09-10 中国科学院化学研究所 Polyacrylic acid printing ink resin and preparation method thereof

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