CN104311728A - Thermoplastic acrylic resin for water transfer printing, preparation method of thermoplastic acrylic resin and water transfer printing ink composition - Google Patents
Thermoplastic acrylic resin for water transfer printing, preparation method of thermoplastic acrylic resin and water transfer printing ink composition Download PDFInfo
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- CN104311728A CN104311728A CN201410621501.1A CN201410621501A CN104311728A CN 104311728 A CN104311728 A CN 104311728A CN 201410621501 A CN201410621501 A CN 201410621501A CN 104311728 A CN104311728 A CN 104311728A
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- acrylic resin
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Abstract
The invention discloses thermoplastic acrylic resin for water transfer printing. The thermoplastic acrylic resin comprises the following raw materials in percentage by weight: 35%-49% of butyl methacrylate and/or butyl acrylate, 1%-15% of methyl acrylate and/or methyl methacrylate, 44%-50% of trimethylbenzene, 2%-6% of tetramethylbenzene, 0.5%-2% of an initiator, 0%-5% of functional acrylic monomers and 0%-7% of styrene. A preparation method of the thermoplastic acrylic resin comprises the following steps: uniformly stirring butyl methacrylate and/or butyl acrylate, methyl acrylate and/or methyl methacrylate, styrene, functional acrylic monomers and part of the initiator to obtain a mixture, dropwise adding the mixture into a mixed reaction solvent of tetramethylbenzene and part of trimethylbenzene with the temperature of 100-110 DEG C, performing heat preservation reaction for 2-3 hours, adding the rest initiator, heating to 110-120 DEG C, keeping on performing heat preservation reaction for 1-3 hours, and adding the rest trimethylbenzene into a reaction material. In addition, the invention further discloses a water transfer printing ink composition containing the thermoplastic acrylic resin. The preparation method is simple, and the prepared resin is high in viscosity, good in adhesion and moderate in hardness.
Description
Technical field
The present invention relates to a kind of acrylic resin, be specifically related to a kind of applicable water transfer printing thermoplastic acrylic resin and preparation method thereof, in addition, the invention still further relates to a kind of water transfer ink composition containing described thermoplastic acrylic resin.
Background technology
At present, the resin used in domestic water transfer printing ink is the solid propenoic acid resin of external import substantially, price is high, uses existing defects, and the second-order transition temperature due to solid propenoic acid resin is 32 DEG C, during summer, the easy melting conglomeration of resin particle, could use dissolution with solvents after need breaking into pieces.And domestic thermoplastic acrylic resin, mostly adopt dimethylbenzene, butylacetate makes solvent, there is irritating smell, be difficult to use in printing industry; And existing thermoplastic acrylic resin, due to molecular weight, causes being difficult to reach balance in hardness and tensile strength.For cost consideration, some producer utilizes acrylic resin to replace acrylic resin in water transfer printing ink, but there is the large defect of fragility, need add toughner and carry out toughness reinforcing, but toughner easily moves, become fragile after causing the water transfer printing marble paper short period of time of producing to be deposited.In addition, the production of existing acrylic resin is the process again to liquid from liquid to solid, more to energy consumption.Therefore, the thermoplastic acrylic resin developing simple, with low cost, the comprehensive use properties of a kind of preparation method good is very necessary.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, the water transfer printing thermoplastic acrylic resin that a kind of preparation method is simple, viscosity is high, sticking power is good, film-forming properties is good is provided; Another object of the present invention is to the preparation method that this thermoplastic acrylic resin a kind of is provided; In addition, present invention also offers a kind of water transfer ink composition containing containing acrylic resin.
For achieving the above object, the present invention is by the following technical solutions:
A kind of water transfer printing thermoplastic acrylic resin, the weight percent of the raw material adopted consists of: butyl methacrylate and/or butyl acrylate 35-49%, methyl acrylate and/or methyl methacrylate 1-15%, trimethylbenzene 44-50%, durene 2-6%, initiator 0.5-2%, functional Acrylic Acid Monomer 0-5%, vinylbenzene 0-7%.
Further: the weight percent of the raw material adopted consists of: butyl methacrylate 38.5%, methyl acrylate 10%, functional Acrylic Acid Monomer 1.5%, initiator 1%, trimethylbenzene 44%, durene 5%.
Preferably: described functional Acrylic Acid Monomer is at least one in stearyl methacrylate, lauryl methacrylate(LMA), isobornyl methacrylate, methyl propenoic acid glycidyl ether.
Preferably: described initiator is at least one in benzoyl peroxide, Diisopropyl azodicarboxylate, peroxidized t-butyl perbenzoate, peroxide acid tert-amyl acetate, di-t-butyl peroxide.
Another object of the present invention, a kind of preparation method of thermoplastic acrylic resin as above, comprises the following steps:
1) using durene and part trimethylbenzene mixing after as reaction solvent;
2) after butyl methacrylate and/or butyl acrylate, methyl acrylate and/or methyl methacrylate, vinylbenzene, functional Acrylic Acid Monomer, part initiator being stirred, for subsequent use;
3) reaction solvent is heated to 100-110 DEG C, then in reaction solvent, evenly drips step 2) in the reaction mass stirred that obtains, reaction mass controls to dropwise in 3-5 hour;
4) step 3) in each material at 100-110 DEG C, continue insulation reaction 2-3 hour after, add residue initiator, and be warming up to 110-120 DEG C continue insulation reaction 1-3 hour;
5) in reaction mass, add remaining trimethylbenzene, obtain described thermoplastic acrylic resin finished product; Wherein:
Step 1) in the consumption of trimethylbenzene be the 50-70% of total trimethylbenzene consumption;
Step 2) in the consumption of initiator be the 50-70% of total initiator amount.
Another object of the present invention, a kind of water transfer ink composition, by weight percentage, composed of the following components: thermoplastic acrylic resin of the present invention: 20-40%, pigment: 40-60%, durene: 10-20%, auxiliary agent: 0.2-1.5%.
Preferably: described auxiliary agent is at least one in dispersion agent, defoamer, flow agent, toughner.
It is even more preferred that described dispersion agent is BYK-192; Described defoamer is BYK-141; Described flow agent is BYK-306 and/or BYK-345; Described toughner is dibutyl phthalate and/or dioctyl phthalate (DOP).
Another object of the present invention, a kind of water transfer ink composition, by weight percentage, composed of the following components: thermoplastic acrylic resin of the present invention: thermoplastic acrylic resin 70-90%; Dyestuff 0.2-1%; Trimethylbenzene 15-30%; Auxiliary agent 0.2-1.5%, wherein, the weight percent summation of each component is 100%.
Preferably: described auxiliary agent be BYK-192, BYK-141, one or more in BYK-306, BYK-345, dibutyl phthalate, dioctyl phthalate (DOP).
Beneficial effect of the present invention is, the problem that it is applied further is limited relative to the molecular weight of current liquid thermoplastic acrylic resin lower (being generally only 6000-15000), the present invention carries out modification with functional Acrylic Acid Monomer to resin, preparation process is simple, the molecular weight of product is controlled by segmentation initiated polymerization, the liquid thermoplastic acrylic resin of number-average molecular weight up to 5-13 ten thousand can be obtained, and obtained acrylic resin to have smell low, viscosity is high, sticking power is good, the feature that hardness is moderate, and resin film forming back draft intensity is good, after 500 DEG C of burnings, ash is few, weathering resistance is strong, be applied in water transfer ink, significantly can promote the over-all properties of ink and reduce the raw materials cost of ink.
Embodiment
Below in conjunction with specific embodiment, the specific embodiment of the present invention is described further.Unless otherwise noted, each raw material adopted in the present invention is all bought by market and is obtained.
Water transfer printing thermoplastic acrylic resin of the present invention, the raw material adopted, by weight percentage, composed of the following components: butyl methacrylate and/or butyl acrylate 35-49%, methyl acrylate and/or methyl methacrylate 1-15%, trimethylbenzene 44-50%, durene 2-6%, initiator 0.5-2%, functional Acrylic Acid Monomer 0-5%, vinylbenzene 0-7%, wherein: described functional Acrylic Acid Monomer is stearyl methacrylate, lauryl methacrylate(LMA), isobornyl methacrylate, one or more in methyl propenoic acid glycidyl ether, described initiator is one or more in benzoyl peroxide, Diisopropyl azodicarboxylate, peroxidized t-butyl perbenzoate, peroxide acid tert-amyl acetate, di-t-butyl peroxide.The preparation process of described thermoplastic acrylic resin comprises the following steps:
1) in reactor, the 50-70% of durene and total trimethylbenzene amount is added as reaction solvent;
2) 50-70% of butyl methacrylate and/or butyl acrylate, methyl acrylate and/or methyl methacrylate, vinylbenzene, functional Acrylic Acid Monomer, total amount of initiator is joined in monomer dropping tank, after stirring, for subsequent use;
3) heat, make reactor constant temperature at 100-110 DEG C, and evenly drip step 2 in reactor) in the reaction mass stirred that obtains, reaction mass controls to dropwise in 3-5 hour;
4) after in reactor, each material continues insulation reaction 2-3 hour at 100-110 DEG C, add residue initiator, and be warming up to 110-120 DEG C continue insulation reaction 1-3 hour, to viscosity 60-90 second/25 DEG C, wherein, described viscosity is the viscosity that form pipe viscometer records;
5) in reactor, add the reaction mass in remaining trimethylbenzene diluting reaction still, obtain thermoplastic acrylic resin finished product of the present invention, after tested, by thermoplastic acrylic resin prepared by above-mentioned component and method, its number-average molecular weight is 5-13 ten thousand, and second-order transition temperature is 20-50 DEG C.
The invention also discloses a kind of water transfer ink containing described thermoplastic acrylic resin, by weight percentage, it consists of: thermoplastic acrylic resin 20-40%, mineral dye 40-60%, durene 10-20%, auxiliary agent 0.2-1.5%; Wherein, described auxiliary agent is at least one in dispersion agent, defoamer, flow agent, toughner, further, and described dispersant B YK-192 (German Bi Ke chemistry, lower same); Described defoamer is BYK-141 (German Bi Ke chemistry, lower same); Described flow agent is BYK-306 (German Bi Ke chemistry, lower same) and/or BYK-345 (German Bi Ke chemistry, lower same); Described toughner is dibutyl phthalate and/or dioctyl phthalate (DOP).By the component of above-mentioned each weight percent composition, be ground to fineness≤20 micron after mixing, obtain a kind of stand linseed oil being applicable to water transfer printing.
The invention also discloses the another kind of water transfer ink containing described thermoplastic acrylic resin, by weight percentage, it consists of: thermoplastic acrylic resin 70-90%; Dyestuff 0.2-1%; Trimethylbenzene 15-30%; Auxiliary agent 0.2-1.5%, the weight percent summation of above each component is 100%; Wherein, described auxiliary agent is at least one in dispersion agent, defoamer, flow agent, toughner, and further, described dispersion agent is BYK-192; Described defoamer is BYK-141; Described flow agent is BYK-306 and/or BYK-345; Described toughner is dibutyl phthalate and/or dioctyl phthalate (DOP).By the component of above-mentioned each weight percent composition, be uniformly mixed under normal temperature, obtain a kind of book binder's ink being applicable to water transfer printing.
Embodiment 1
A kind of water transfer printing thermoplastic acrylic resin, raw materials used weight percent consists of: butyl methacrylate 38.5%, methyl acrylate 10%, stearyl methacrylate 1.5%, di-t-butyl peroxide 1%, trimethylbenzene 44%, durene 5%; Its preparation process comprises the following steps:
1) in reactor, 50% of the durene of above-mentioned weight percent and total trimethylbenzene amount is added as reaction solvent;
2) by the butyl methacrylate of above-mentioned weight percent, methyl acrylate, stearyl methacrylate and in di-t-butyl peroxide amount 60%, after being uniformly mixed under normal temperature, for subsequent use;
3) reacting by heating still when still internal solvent reaches 100 DEG C, evenly drips step 2 in reactor) in the reaction mass stirred that obtains, reaction mass controls to dropwise in 3 hours;
4) in reactor, each material continued insulation reaction after 1 hour at 100 DEG C, added residue initiator di-t-butyl peroxide, and it is little qualified up to viscosity to be warming up to 115 DEG C of continuation insulation reaction 2;
5) in reactor, add the reaction mass in remaining trimethylbenzene diluting reaction still, obtain thermoplastic acrylic resin finished product of the present invention.
Embodiment 2
A kind of water transfer printing thermoplastic acrylic resin, raw materials used weight percent consists of: butyl acrylate 38%, methyl methacrylate 5%, vinylbenzene 5%, isobornyl acrylate 2%, di-t-butyl peroxide 2%, trimethylbenzene 45%, durene 3%, its preparation process is with embodiment 1.
Carry out performance test to thermoplastic acrylic resin obtained in above-described embodiment 1, its detected result is as shown in table 1:
Table 1 thermoplastic acrylic resin performance test results
| Project | Index | Detected result | Examination criteria |
| Outward appearance | Clear viscous fluid | Meet | GB/T?1721-2008 |
| Molecular weight (number all) | ＞20000 | 85000 | Gel permeation chromatography |
| Second-order transition temperature/DEG C | - | 30℃ | Differential scanning amount thermal analyses (DSC) method |
| Solid content (150 DEG C × 2h) % | 48～50％ | 49.35％ | GB/T?1725-2007 |
| Color and luster (FeCo) | ≤1# | 1# | GB/T?1722-1992 |
| Viscosity/second (25 DEG C, form viscosity) | 60～90 | 82 | GB/T?1723-1993 |
| Fineness | ≤20μm | 20μm | GB/T?1724-1979 |
As known from Table 1, the thermoplastic acrylic resin that the present invention obtains, its outward appearance is clear viscous liquid, 6000-15000 is only relative to the molecular weight of current liquid thermoplastic acrylic resin, the molecular weight of thermoplastic acrylic resin of the present invention can reach 5-13 ten thousand, and color and luster is good, viscosity is high, and decomposition temperature is below 500 DEG C, ash after incineration is little, stay in grade.
Embodiment 3
A kind of water transfer ink composition, by weight percentage, composed of the following components: thermoplastic acrylic resin obtained in embodiment 1: 35%, iron oxide red: 50%, durene: 14%, BYK-192:0.2%, BYK-141:0.1%, BYK345:0.3%, dibutyl phthalate: 0.4%, after each component is uniformly mixed under normal temperature by above-mentioned weight percent, be ground to fineness≤20 micron, obtain a kind of stand linseed oil being applicable to water transfer printing.
Embodiment 4
A kind of water transfer ink composition, by weight percentage, composed of the following components: thermoplastic acrylic resin 80% obtained in embodiment 2, dyestuff Huang 0.8%, trimethylbenzene 18%, BYK-192:0.4%, BYK-306:0.5%, dioctyl phthalate (DOP): 0.3%; After each component being uniformly mixed under normal temperature by above-mentioned weight percent, obtain a kind of book binder's ink being applicable to water transfer printing.
Specific embodiment described in the invention is only for the detailed description of the specific implementation process to this water transfer printing thermoplastic acrylic resin and the water transfer ink containing this acrylic resin, instead of the restriction to its preparation method.Any modification of carrying out this product and improvement, the substituting and using of similar or close material in the scope of the claims or category, all belongs to scope of patent protection of the present invention.
Claims (10)
1. a water transfer printing thermoplastic acrylic resin, is characterized in that: the weight percent of the raw material adopted consists of: butyl methacrylate and/or butyl acrylate 35-49%, methyl acrylate and/or methyl methacrylate 1-15%, trimethylbenzene 44-50%, durene 2-6%, initiator 0.5-2%, functional Acrylic Acid Monomer 0-5%, vinylbenzene 0-7%.
2. thermoplastic acrylic resin according to claim 1, is characterized in that: the weight percent of the raw material adopted consists of: butyl methacrylate 38.5%, methyl acrylate 10%, functional Acrylic Acid Monomer 1.5%, initiator 1%, trimethylbenzene 44%, durene 5%.
3. thermoplastic acrylic resin according to claim 1 and 2, is characterized in that: described functional Acrylic Acid Monomer is at least one in stearyl methacrylate, lauryl methacrylate(LMA), isobornyl methacrylate, methyl propenoic acid glycidyl ether.
4. thermoplastic acrylic resin according to claim 1 and 2, is characterized in that: described initiator is at least one in benzoyl peroxide, Diisopropyl azodicarboxylate, peroxidized t-butyl perbenzoate, peroxide acid tert-amyl acetate, di-t-butyl peroxide.
5. a preparation method for thermoplastic acrylic resin as claimed in claim 1 or 2, is characterized in that: comprise the following steps:
1) using durene and part trimethylbenzene mixing after as reaction solvent;
2) after butyl methacrylate and/or butyl acrylate, methyl acrylate and/or methyl methacrylate, vinylbenzene, functional Acrylic Acid Monomer, part initiator being stirred, for subsequent use;
3) reaction solvent is heated to 100-110 DEG C, then in reaction solvent, evenly drips step 2) in the reaction mass stirred that obtains, reaction mass controls to dropwise in 3-5 hour;
4) step 3) in each material at 100-110 DEG C, continue insulation reaction 2-3 hour after, add residue initiator, and be warming up to 110-120 DEG C continue insulation reaction 1-3 hour;
5) in reaction mass, add remaining trimethylbenzene, obtain described thermoplastic acrylic resin finished product.
6. a water transfer ink composition, it is characterized in that: by weight percentage, composed of the following components: the thermoplastic acrylic resin according to any one of claim 1-4: 20-40%, pigment: 40-60%, durene: 10-20%, auxiliary agent: 0.2-1.5%.
7. water transfer ink composition according to claim 6, is characterized in that: described auxiliary agent is at least one in dispersion agent, defoamer, flow agent, toughner.
8. water transfer ink composition according to claim 7, is characterized in that: described dispersion agent is BYK-192; Described defoamer is BYK-141; Described flow agent is BYK-306 and/or BYK-345; Described toughner is dibutyl phthalate and/or dioctyl phthalate (DOP).
9. a water transfer ink composition, is characterized in that: by weight percentage, composed of the following components: the thermoplastic acrylic resin in claim 1-4 described in any one: thermoplastic acrylic resin 70-90%; Dyestuff 0.2-1%; Trimethylbenzene 15-30%; Auxiliary agent 0.2-1.5%, wherein, the weight percent summation of each component is 100%.
10. water transfer ink composition according to claim 9, is characterized in that: described auxiliary agent is one or more in BYK-192, BYK-141, BYK-306, BYK-345, dibutyl phthalate, dioctyl phthalate (DOP).
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104945808A (en) * | 2015-07-16 | 2015-09-30 | 田菱精密制版（深圳）有限公司 | Cover oil resin combination used for hydrographics transfer printing |
| CN104974310A (en) * | 2015-06-12 | 2015-10-14 | 长沙市汇华胶粘剂科技有限公司 | Resin for peelable membrane oil of water sticking paper and preparation method thereof |
| CN106188381A (en) * | 2016-08-09 | 2016-12-07 | 王建周 | A kind of flame-proofed thermoplastic acrylic acid resin composition and preparation method thereof |
| CN106752314A (en) * | 2016-12-08 | 2017-05-31 | 博立尔化工（扬州）有限公司 | A kind of UV cured printing inks |
| CN111303336A (en) * | 2020-03-13 | 2020-06-19 | 广东鲸鲨化工有限公司 | Water transfer printing tearable film resin, preparation method thereof and water transfer printing tearable film composition |
| CN114149531A (en) * | 2021-11-18 | 2022-03-08 | 南雄西顿化工有限公司 | Water-based acrylic resin capable of transferring and printing gloss oil and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104974310A (en) * | 2015-06-12 | 2015-10-14 | 长沙市汇华胶粘剂科技有限公司 | Resin for peelable membrane oil of water sticking paper and preparation method thereof |
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| CN106752314A (en) * | 2016-12-08 | 2017-05-31 | 博立尔化工（扬州）有限公司 | A kind of UV cured printing inks |
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| CN114149531A (en) * | 2021-11-18 | 2022-03-08 | 南雄西顿化工有限公司 | Water-based acrylic resin capable of transferring and printing gloss oil and preparation method thereof |
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| CN104311728B (en) | 2016-08-24 |
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Address after: 528100 "National Torch Plan Foshan Electronics and Electrical Industry Base" No. 114, South District, Baini Town, Sanshui District, Foshan City, Guangdong Province (F6) Patentee after: Guangdong Whale Shark Chemical Co., Ltd. Address before: 528100 "National Torch Plan Foshan Electronics and Electrical Industry Base" No. 114, South District, Baini Town, Sanshui District, Foshan City, Guangdong Province (F6) Patentee before: FOSHAN JINGSHA CHEMICAL CO., LTD. |