CN101747475B - Formulation of synthetic resin for alcohol-soluble printing ink and preparation method thereof - Google Patents
Formulation of synthetic resin for alcohol-soluble printing ink and preparation method thereof Download PDFInfo
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- CN101747475B CN101747475B CN 200810188225 CN200810188225A CN101747475B CN 101747475 B CN101747475 B CN 101747475B CN 200810188225 CN200810188225 CN 200810188225 CN 200810188225 A CN200810188225 A CN 200810188225A CN 101747475 B CN101747475 B CN 101747475B
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Abstract
The invention relates to a resin for alcohol-soluble printing ink and relates to the field of chemical synthesis. The current plastic gravure ink uses a benzene-soluble synthetic resin as a main part, so volatilization pollution of a benzene solvent exists in manufacturing and using processes of the printing ink and endangers the health of human body. The invention provides a formulation of the resin for the alcohol-soluble printing ink and a preparation method thereof. The preparation method comprises the following steps: using acrylic ester, ethylene carbonate, vinyl acetate and an active functional group monomer as raw materials; adding an initiator to the raw materials; dissolving the mixture in mixed solution; under a stirring condition, dripping mixture solution of the monomer and a solvent in an alcohol ester solvent to prepare an acrylic pre-polymer; using the solvent to fully dissolve a condensation polymer of cyclohexanone and formaldehyde; under the stirring condition, adding a catalyst and the acrylic pre-polymer; performing a reaction between the dissolved condensation polymer and the acrylic pre-polymer to an end point; lowering the temperature; and adjusting the viscosity to obtain a finished product. The resin is alcohol soluble and has little harm to the human body and the environment. Moreover, the resin has the characteristics of convenient and readily available raw materials, low preparation cost, good pigment-wetting dispersivity and high drying speed.
Description
Technical field
The present invention relates to the synthetic field of chemical industry, relate in particular to prescription of a kind of synthetic resin for alcohol-soluble printing ink and preparation method thereof.
Background technology
Plastic gravure printing ink is the coloured material that is used for the plastic wrapping printing.Be to be main component by resin, solvent, pigment and auxiliary agent, through the liquid substance that working procedure processing such as grindings form, wherein the performance of resin determines the printing ink solvent type; And the printability, pigment-dispersing, attachment fastness etc. of decision printing ink; For a long time, the plastic gravure printing ink of China dissolves type synthetic resins with benzene and is the main body, contains a large amount of benzene kind solvents in the printing ink; Pollute the health that is endangering the producer and human consumer so all exist the volatilization of benzene solvent in the manufacturing of printing ink, the use.Even more serious is the benzene kind solvent that remains in the packing bag, is polluting article, food, very big to the people's lives Health hazard.In recent years, though occur the alcohol-soluble printing ink of water-based, alcohol-soluble polyurethane plastic gravure printing ink and other type in the market, exist price high; To the pigment wetting bad dispersibility; Drying waits problem slowly, has influenced promoting the use of of this series products, at acrylic acid or the like associated resin and printing ink; Still there are minority one or two tame products to be able to use with regard to white single kind is domestic, but present domestic this resinoid supply of still not having of the pure dissolubility plastic gravure printing ink of whole chromatogram.
Summary of the invention
The objective of the invention is a kind of ethanol-soluble type synthetic resins and compound method, satisfy ethanol-soluble type compound oil ink whole chromatogram and make requirement.
The technical scheme that realizes above-mentioned purpose is following:
A kind of synthetic resin for alcohol-soluble printing ink, fill a prescription as follows:
75 parts of polycondensate 30-35 part, catalyzer 0.5-0.7 part, butylacetate 20-25 part, ETHYLE ACETATE 10-15 part, the absolute ethyl alcohols of propenoate 24-39 part, tertiary ethylene carbonate 5-10 part, vinyl-acetic ester 15-20 part, active function groups monomer 15-21 part, initiator 0.5-0.7 part, pimelinketone and formaldehyde.
Described propenoate is one or more in ethyl propenoate, Bing Xisuandingzhi, the NSC 20956; Described active function groups monomer is one or more the mixture in vinylformic acid, propenoic acid beta hydroxyl ethyl ester, Propylene glycol monoacrylate, glycidyl acrylate, the acrylic amide; Described initiator is an azobisisobutyronitrile, and described catalyzer is a tosic acid.
The preparation method of synthetic resin for alcohol-soluble printing ink is made up of following steps:
(1) ETHYLE ACETATE 5-10 part and absolute ethyl alcohol are mixed in the adding reaction kettle for 45 parts, make pure ester solvent, subsequent use;
(2) propenoate 24-39 part, tertiary ethylene carbonate 5-10 part, vinyl-acetic ester 15-20 part, active function groups monomer 15-21 part, initiator 0.5-0.7 part are dissolved in the mixing solutions of 10 parts of ETHYLE ACETATE 5-10 parts, absolute ethyl alcohol; Make monomer mixed solution, and place header tank subsequent use;
(3) under agitation condition, the monomer mixed solution that step (2) is made is added drop-wise in the pure ester solvent that step (1) makes, and the dropping time is 3-4 hour, drips to finish back backflow 1-2 hour, and temperature of reaction is 72-78 ℃, makes the acrylic acid multielement performed polymer, and is subsequent use;
(4) in another reaction kettle, add butylacetate 20-25 part, under agitation condition polycondensate 30-35 part of adding pimelinketone and formaldehyde; Be warming up to 65 ℃ it is dissolved fully, add the acrylic acid multielement performed polymer that catalyzer 0.5-0.7 part and step (3) make while stirring, temperature is controlled at 95-98 ℃; React to terminal with acrylate prepolymer; Be cooled to 65 ℃, add 20 parts of absolute ethyl alcohol adjustment viscosity, discharging makes finished product.
The synthetic resin for alcohol-soluble printing ink that the present invention makes is pure dissolubility, does not use benzene kind solvent, and is little to human body, environmental hazard.
Raw material of the present invention conveniently is easy to get, and preparation cost is low.
The present invention also has the pigment wetting good dispersivity, the characteristics of fast drying.
Embodiment
With embodiment the present invention is done further explanation below, but the present invention is not restricted to following embodiment.
Embodiment 1
Prescription is:
10 parts in 20 parts of 0.5 part of 30 parts of polycondensates, tosic acid, butylacetates, the ETHYLE ACETATE of 15 parts of methylacrylic acid ester methyl esters, 16 parts of ethyl propenoates, 8 parts of NSC 20956s, 5 parts of tertiary ethylene carbonates, 15 parts of vinyl-acetic esters, 2 parts in vinylformic acid, 5 parts of Propylene glycol monoacrylates, 8 parts of acrylic amides, 0.5 part of azobisisobutyronitrile, pimelinketone and formaldehyde, 75 parts of absolute ethyl alcohols.
The preparation method is made up of following steps:
(1) 5 parts in ETHYLE ACETATE and absolute ethyl alcohol are mixed in the adding reaction kettle for 45 parts, make 50 parts of pure ester solvents, subsequent use;
(2) 0.5 part of 15 parts of methylacrylic acid ester methyl ester, 16 parts of ethyl propenoates, NSC 20956 .8 part, 5 parts of tertiary ethylene carbonates, 15 parts of vinyl-acetic esters, 2 parts in vinylformic acid, 5 parts of Propylene glycol monoacrylates, 8 parts of acrylic amides, azobisisobutyronitrile is dissolved in the mixing solutions of 5 parts in ETHYLE ACETATE, 10 parts of absolute ethyl alcohols; Make monomer mixed solution, and place header tank subsequent use;
(3) under agitation condition, the monomer mixed solution that step (2) is made is added drop-wise in the pure ester solvent that step (1) makes, and the dropping time is 3 hours, drips to finish the back and refluxed 1 hour, and temperature of reaction is 72 ℃, makes the acrylic acid multielement performed polymer, and is subsequent use;
(4) in another reaction kettle, add 20 parts of butylacetates, under agitation condition 30 parts of the polycondensates of adding pimelinketone and formaldehyde; Be warming up to 65 ℃ it is dissolved fully, add the acrylic acid multielement performed polymer that 0.5 part of benzene methanesulfonic acid and step (3) are made while stirring, temperature is controlled at 95 ℃; React to terminal with acrylate prepolymer; Be cooled to 65 ℃, add 20 parts of absolute ethyl alcohol adjustment viscosity, discharging makes finished product.
Embodiment 2
Prescription is: 10 parts in 20 parts of 0.5 part of 0.7 part of 30 parts of polycondensates, azobisisobutyronitrile, tosic acid, butylacetates, the ETHYLE ACETATE of 5 parts of methylacrylic acid ester methyl esters, 19 parts of NSC 20956s, 20 parts of vinyl-acetic esters, 10 parts of tertiary ethylene carbonates, 3 parts in vinylformic acid, 4 parts of propenoic acid beta hydroxyl ethyl esters, 2 parts of glycidyl acrylates, 11 parts of acrylic amides, pimelinketone and formaldehyde, 75 parts of absolute ethyl alcohols
The preparation method is made up of following steps:
(1) 5 parts in ETHYLE ACETATE and absolute ethyl alcohol are mixed in the adding reaction kettle for 45 parts, make 50 parts of pure ester solvents, subsequent use;
(2) 0.7 part of 5 parts of methylacrylic acid ester methyl ester, 19 parts of NSC 20956s, 20 parts of vinyl-acetic esters, 10 parts of tertiary ethylene carbonates, 3 parts in vinylformic acid, 4 parts of propenoic acid beta hydroxyl ethyl esters, 2 parts of glycidyl acrylates, 11 parts of acrylic amides, azobisisobutyronitrile is dissolved in the mixing solutions of 5 parts in ETHYLE ACETATE, 10 parts of absolute ethyl alcohols; Make monomer mixed solution, and place header tank subsequent use;
(3) under agitation condition, the monomer mixed solution that step (2) is made is added drop-wise in the pure ester solvent that step (1) makes, and the dropping time is 3.5 hours, drips to finish the back and refluxed 1.5 hours, and temperature of reaction is 75 ℃, makes the acrylic acid multielement performed polymer, and is subsequent use;
(4) in another reaction kettle, add 30 parts of the polycondensates of 20 parts of butylacetates, pimelinketone and formaldehyde, 30 parts of the polycondensates of adding pimelinketone and formaldehyde are warming up to 65 ℃ it are dissolved fully under agitation condition; Agitation condition adds the acrylic acid multielement performed polymer that 0.5 part of tosic acid and step (3) make down; Temperature is controlled at 96 ℃, reacts to terminal with acrylate prepolymer, is cooled to 65 ℃; Add 20 parts of absolute ethyl alcohols, discharging makes finished product.
Embodiment 3
Prescription is:
15 parts in 25 parts of 0.7 part of 1 part of 35 parts of polycondensates, initiator, catalyzer, butylacetates, the ETHYLE ACETATE of 6 parts of ethyl propenoates, 25 parts of NSC 20956s, 5 parts of tertiary ethylene carbonates, 20 parts of vinyl-acetic esters, 3 parts in vinylformic acid, 5 parts of propenoic acid beta hydroxyl ethyl esters, 3 parts of glycidyl acrylates, 10 parts of acrylic amides, pimelinketone and formaldehyde, 75 parts of absolute ethyl alcohols.
(1) 8 parts in ETHYLE ACETATE and absolute ethyl alcohol are mixed in the adding reaction kettle for 45 parts, make 53 parts of pure ester solvents, subsequent use;
(2) 1 part of 6 parts of ethyl propenoate, 25 parts of NSC 20956s, 5 parts of tertiary ethylene carbonates, 20 parts of vinyl-acetic esters, 3 parts in vinylformic acid, 5 parts of propenoic acid beta hydroxyl ethyl esters, 3 parts of glycidyl acrylates, 10 parts of acrylic amides, azobisisobutyronitrile is dissolved in the mixing solutions of 7 parts in ETHYLE ACETATE, 10 parts of absolute ethyl alcohols; Make monomer mixed solution, and place header tank subsequent use;
(3) under agitation condition, the monomer mixed solution that step (2) is made is added drop-wise in the pure ester solvent that step (1) makes, and the dropping time is 4 hours, drips to finish the back and refluxed 2 hours, and temperature of reaction is 78 ℃, makes the acrylic acid multielement performed polymer, and is subsequent use;
(4) in another reaction kettle, add 35 parts of the polycondensates of 25 parts of butylacetates, pimelinketone and formaldehyde, 30 parts of the polycondensates of adding pimelinketone and formaldehyde are warming up to 65 ℃ it are dissolved fully under agitation condition; Add the acrylic acid multielement performed polymer that 0.7 part of tosic acid and step (3) make while stirring; Temperature is controlled at 98 ℃, reacts to terminal with acrylate prepolymer, is cooled to 65 ℃; Add 20 parts of absolute ethyl alcohols, discharging makes finished product.
Claims (2)
1. synthetic resin for alcohol-soluble printing ink; It is characterized by prescription as follows: 75 parts of 10-15 parts in 20-25 parts of 0.5-0.7 part of 30-35 parts of polycondensates, catalyzer, butylacetates, the ETHYLE ACETATE of 24-39 parts of propenoate, 5-10 parts of tertiary ethylene carbonates, 15-20 parts of vinyl-acetic esters, 15-21 parts of active function groups monomers, 0.5-0.7 part of initiator, pimelinketone and formaldehyde, absolute ethyl alcohols
Preparation according to the following steps:
(1) 5-10 parts in ETHYLE ACETATE and absolute ethyl alcohol are mixed in the adding reaction kettle for 45 parts, make pure ester solvent, subsequent use;
(2) 0.5-0.7 part of 24-39 parts of propenoate, 5-10 parts of tertiary ethylene carbonates, 15-20 parts of vinyl-acetic esters, 15-21 parts of active function groups monomers, initiator is dissolved in the mixing solutions of 5-10 parts in ETHYLE ACETATE, 10 parts of absolute ethyl alcohols; Make monomer mixed solution, and place header tank subsequent use;
(3) under agitation condition, the monomer mixed solution that step (2) is made is added drop-wise in the pure ester solvent that step (1) makes, and the dropping time is 3-4 hours; Drip and finish back backflow 1-2 hours; Temperature of reaction is 72-78 ℃, makes the acrylic acid multielement performed polymer, and is subsequent use;
(4) in another reaction kettle, add 20-25 parts of butylacetates, under agitation condition 30-35 parts of the polycondensates of adding pimelinketone and formaldehyde, be warming up to 65 ℃ it dissolved fully, add the acrylic acid multielement performed polymer that 0.5-0.7 part of catalyzer and step (3) make while stirring; Temperature is controlled at 95-98 ℃; With the acrylic acid multielement prepolymer reaction to terminal, be cooled to 65 ℃, add 20 parts of absolute ethyl alcohols adjustment viscosity; Discharging makes finished product
Wherein, said active function groups monomer is one or more the mixture in vinylformic acid, propenoic acid beta hydroxyl ethyl ester, Propylene glycol monoacrylate, glycidyl acrylate, the acrylic amide.
2. a kind of synthetic resin for alcohol-soluble printing ink according to claim 1; It is characterized in that described propenoate is one or more in ethyl propenoate, Bing Xisuandingzhi, the NSC 20956; Described initiator is a Diisopropyl azodicarboxylate, and described catalyzer is a tosic acid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810188225 CN101747475B (en) | 2008-12-19 | 2008-12-19 | Formulation of synthetic resin for alcohol-soluble printing ink and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200810188225 CN101747475B (en) | 2008-12-19 | 2008-12-19 | Formulation of synthetic resin for alcohol-soluble printing ink and preparation method thereof |
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| Publication Number | Publication Date |
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| CN101747475A CN101747475A (en) | 2010-06-23 |
| CN101747475B true CN101747475B (en) | 2012-10-10 |
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| CN 200810188225 Expired - Fee Related CN101747475B (en) | 2008-12-19 | 2008-12-19 | Formulation of synthetic resin for alcohol-soluble printing ink and preparation method thereof |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102344540B (en) * | 2011-08-04 | 2013-01-09 | 北京高盟新材料股份有限公司 | Preparation method of heat resistance resin used for printing ink |
| CN103183786B (en) * | 2011-12-29 | 2016-01-13 | 德谦（上海）化学有限公司 | The spirit-soluble resin that a kind of look ink is general |
| CN102718916B (en) * | 2012-06-15 | 2014-04-16 | 北京高盟新材料股份有限公司 | Alcohol-water-soluble vinyl versatate modified vinegar C system acrylic resin and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002302894A (en) * | 2001-01-30 | 2002-10-18 | Sekisui Chem Co Ltd | Emulsion-type adhesive for water-repellent paper |
| CN1737021A (en) * | 2005-07-15 | 2006-02-22 | 邹文俊 | Alcohol-soluble resin and its preparation method |
| CN101230220A (en) * | 2007-12-26 | 2008-07-30 | 宁波工程学院 | Emulsion bridging agent for aqueous ink and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002302894A (en) * | 2001-01-30 | 2002-10-18 | Sekisui Chem Co Ltd | Emulsion-type adhesive for water-repellent paper |
| CN1737021A (en) * | 2005-07-15 | 2006-02-22 | 邹文俊 | Alcohol-soluble resin and its preparation method |
| CN101230220A (en) * | 2007-12-26 | 2008-07-30 | 宁波工程学院 | Emulsion bridging agent for aqueous ink and preparation method thereof |
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Granted publication date: 20121010 Termination date: 20131219 |