CN103122050A - Synthetic resin for water-soluble printing ink and preparation method thereof - Google Patents
Synthetic resin for water-soluble printing ink and preparation method thereof Download PDFInfo
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- CN103122050A CN103122050A CN2013100599348A CN201310059934A CN103122050A CN 103122050 A CN103122050 A CN 103122050A CN 2013100599348 A CN2013100599348 A CN 2013100599348A CN 201310059934 A CN201310059934 A CN 201310059934A CN 103122050 A CN103122050 A CN 103122050A
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Abstract
The invention belongs to the field of synthetic resin and provides synthetic resin for water-soluble printing ink. The synthetic resin is prepared from 15-21 parts of turpentine oil, 15-45 parts of butyl acrylate, 7-15 parts of methyl methacrylate or styrene, 20-35 parts of vinyl acetate and 6-12 parts of active functional group monomer. A preparation method comprises the following steps of: reacting the turpentine oil under the effect of a mixed catalyst of benzyl chloride and aluminum chloride to obtain a terpene prepolymer; making the terpene prepolymer into an emulsion; adding butyl acrylate, methyl methacrylate, vinyl acetate and part of the active functional group monomer into the terpene prepolymer emulsion; adding part of an initiator and the remaining monomer mixture at 60-80 DEG C, and reacting for 10-20 minutes; adding the remaining initiator and heating to 90-95 DEG C for reaction; and cooling to obtain the synthetic resin for water-soluble printing ink.
Description
Technical field
The invention belongs to the synthetic resins field, be specifically related to the synthetic resins that a kind of water-based ink is used, and preparation method thereof.
Background technology
plastic gravure printing ink is the coloured material of plastic wrapping printing, by resin, solvent, pigment and auxiliary agent are Main Components, the liquid substance that processes through operations such as grindings, wherein the performance of resin determines the printing ink solvent type, and the printability of decision printing ink, pigment-dispersing, attachment fastness etc., for a long time, the plastic gravure printing ink of China is take benzene and other organic molten type synthetic resins as main body, contain a large amount of benzene classes and other organic solvent in printing ink, so manufacturing of printing ink, the volatilization that all exists benzene solvent and other organic solvent in use procedure is polluted, endangering the producer and human consumer's health.More seriously remain in benzene and other organic solvent in packing bag, polluting article, food, very large to the people's lives Health hazard.In recent years, although occur the printing ink of water-based plastic gravure ink and other type in market, exist price high, to pigment wetting bad dispersibility, the problem such as dry slow, attachment fastness is poor, affected promoting the use of of this series products.
Summary of the invention
The purpose of this invention is to provide a kind of water-based ink synthetic resins, with the pollution of avoiding using benzene and other organic solvent to be caused.
Another object of the present invention is to provide the preparation method that described water-based ink is used synthetic resins.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is as follows:
Water-based ink comprises the steps: with the preparation method of synthetic resins
(1) turps is dissolved in organic solvent, then adds catalyzer to react under 5～15 ℃ 1～5 hour, described catalyzer is the mixture of Benzyl Chloride and aluminum chloride;
(2) add water in the reaction solution of step (1), stir, filter, the filtrate standing demix obtains organic layer, and organic layer washes with water to neutrality, then steaming obtains the terpenes prepolymer except organic solvent;
(3) terpenes prepolymer and emulsifying agent are added to the water, heated and stirred is made the terpenes pre-polymer emulsion;
(4) butyl acrylate, methyl methacrylate, vinyl-acetic ester and active function groups monomer are mixed to get monomer mixture;
(5) being added in the terpenes pre-polymer emulsion the first part of monomer mixture, after heated and stirred is even, under 60～80 ℃, partly initiator and remaining monomer mixture are added again, react after 10～20 minutes, again remaining initiator is added, then be warming up to 90～95 ℃ of reactions 20～40 minutes, cooling.
Further, the mixture of described organic solvent ethyl acetate and toluene.
Further, described catalyzer is 1:(0.5～2 by weight by Benzyl Chloride and aluminum chloride) form; Preferred weight ratio is 1:1.
Further, the consumption of described catalyzer is 2.5～7.5% of turps weight.
Further, described emulsifying agent is the mixture of OP-10 and Sodium dodecylbenzene sulfonate.
Further, emulsifying agent is (1～3) by weight by OP-10 and Sodium dodecylbenzene sulfonate: 1 forms; Preferred weight ratio is 2:1.
Further, the consumption of described emulsifying agent is 3～8% of turps weight.
Further, count by weight, during preparation, the consumption of raw material is as follows: 15～21 parts, turps, 15～45 parts of butyl acrylates, 7～15 parts of methyl methacrylates, 20～35 parts of vinyl-acetic esters, 6～12 parts of active function groups monomers, 0.35～0.6 part of initiator.
Further, described active function groups monomer is at least a in vinylformic acid, methacrylic acid, Hydroxyethyl acrylate, Propylene glycol monoacrylate, tertiary ethylene carbonate and glycidyl acrylate.
Further, described initiator is persulphate.
Further, the preferred Potassium Persulphate of described persulphate, Sodium Persulfate or ammonium persulphate, preferred persulphate are vitriolate of tartar.
Further, be to add by 1/3～2/3 of monomer mixture total amount the adding of monomer mixture part described in step (5), and the initiator of described part refers to that add-on is 1/3～2/3 of initiator total amount.
Further, in above-mentioned preparation method, described methyl methacrylate can replace with vinylbenzene.
Beneficial effect: adopting the prepared synthetic resins of aforesaid method is water-based emulsion, do not contain benzene and other organic solvent, can be used for producing the plastics aquosity intaglio printing ink, to human body, environmentally friendly, and have that raw material conveniently is easy to get, preparation cost is low, adhesion strength is high, the characteristics of pigment wetting good dispersity, fast drying.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
α-pinene content 〉=78% in the present invention's turps used, beta-pinene 〉=15%, boiling range: 155～170 ℃.
Embodiment 1
Preparation water-based ink raw materials used consumption during with synthetic resins: 210 kilograms, turps, 290 kilograms of butyl acrylates, 70 kilograms of methyl methacrylates, 350 kilograms of vinyl-acetic esters, 50 kilograms of Hydroxyethyl acrylates, 30 kilograms, vinylformic acid, 4.8 kilograms of Potassium Persulphates, catalyzer: 5.5 kilograms, the mixture of Benzyl Chloride and aluminum chloride (mass ratio is 1:1).
Water-based ink is as follows with the concrete preparation process of synthetic resins:
1. terpenes prepolymer preparation
[1] catalyzer is added in the mixed solvent that is formed by 36kg ethyl acetate and 4kg toluene mixing;
[2] drop into reactor with turps with by the mixed solvent that 162kg ethyl acetate and 18kg toluene form, stir;
[3] when temperature of reaction kettle reaches 5 ℃, the catalyst solution of step [1] gained is added in reactor, keep temperature of reaction kettle and be no more than 15 ℃, reacted 3 hours;
[4] 200kg hot water (temperature is 75 ℃) is added reactor carry out the hot water hydrolysis, stir after 20 minutes, solids removed by filtration impurity, the filtrate standing demix, get organic phase and with hot water wash to neutral Zai＜=0.015MPa, temperature is that under 75-85 ℃, decompression steams organic solvent and residual reactant, obtains the terpenes prepolymer;
[5] 900kg water, emulsifying agent 6.5kg (OP-10 is 2:1 with the mass ratio of Sodium dodecylbenzene sulfonate) are mixed with the terpenes prepolymer, stirring is warming up to 50 ℃ of emulsifications and obtains the terpenes pre-polymer emulsion, and is standby;
[6] with the initiator (Potassium Persulphate) of 100kg water and 4.8kg, add in dissolving vessel, be stirred to dissolving fully, obtain initiator solution;
[7] butyl acrylate, methyl methacrylate, vinyl-acetic ester, Hydroxyethyl acrylate and vinylformic acid are mixed, obtain monomer mixture;
[8] first 1/3 monomer mixture of measuring is added in the terpenes pre-polymer emulsion, stirring and evenly mixing, when being warming up to 70 ℃ under agitation condition, the monomer mixture of the amount of 2/3 under remaining with 1.5～2 hours again and the initiator solution of 2/3 amount splash into, and monomer mixture and initiator solution are synchronously dripped off, be incubated after 10 minutes, splash into the initiator solution of remaining 1/3 amount, dripped off with 20-30 minute, below temperature-stable to 80 ℃, be warming up to 90-95 ℃ after dripping, insulation 30min, vacuumize (＜=0.015MPa) and remove the complete monomer of unreacted, cooling, add the ammoniacal liquor adjust pH to 8-8.5, discharging.
Embodiment 2
Preparation water-based ink raw materials used consumption during with synthetic resins: 180 kilograms, turps, 380 kilograms of butyl acrylates, methyl methacrylate double centner, 270 kilograms of vinyl-acetic esters, 40 kilograms of glycidyl acrylates, 30 kilograms, vinylformic acid, 5.1 kilograms of Potassium Persulphates, catalyzer: 4.8 kilograms, the mixture of Benzyl Chloride and aluminum chloride (mass ratio is 1:1).
Water-based ink is as follows with the concrete preparation process of synthetic resins:
1. terpenes prepolymer preparation
[1] catalyzer is added in the mixed solvent that is formed by 36kg ethyl acetate and 4kg toluene mixing;
[2] drop into reactor with turps with by the mixed solvent that 135kg ethyl acetate and 18kg toluene form, stir;
[3] when temperature of reaction kettle reaches 10 ℃, the catalyst solution of step [1] gained is added in reactor, keep temperature of reaction kettle and be no more than 15 ℃, reacted 3 hours;
[4] 200kg hot water (temperature is 85 ℃) is added reactor carry out the hot water hydrolysis, stir after 10 minutes, solids removed by filtration impurity, the filtrate standing demix, get organic phase and with hot water wash to neutral Zai＜=0.015MPa, temperature is that under 75-85 ℃, decompression steams organic solvent and residual reactant, obtains the terpenes prepolymer;
[5] 900kg water, emulsifying agent 6.5kg (OP-10 is 2:1 with the mass ratio of Sodium dodecylbenzene sulfonate) are mixed with the terpenes prepolymer, stirring is warming up to 50 ℃ of emulsifications and obtains the terpenes pre-polymer emulsion, and is standby;
[6] with the initiator (Potassium Persulphate) of 100kg water and 5.1kg, add in dissolving vessel, be stirred to dissolving fully, obtain initiator solution;
[7] butyl acrylate, methyl methacrylate, vinyl-acetic ester, glycidyl acrylate and vinylformic acid are mixed, obtain monomer mixture;
[8] first 1/3 monomer mixture of measuring is added in the terpenes pre-polymer emulsion, stirring and evenly mixing, when being warming up to 80 ℃ under agitation condition, the monomer mixture of the amount of 2/3 under remaining with 1.5～2 hours again and the initiator solution of 2/3 amount splash into, and monomer mixture and initiator solution are synchronously dripped off, be incubated after 10 minutes, splash into the initiator solution of remaining 1/3 amount, dripped off with 20-30 minute, below temperature-stable to 80 ℃, be warming up to 90-95 ℃ after dripping, insulation 30min, vacuumize (＜=0.015MPa) and remove the complete monomer of unreacted, cooling, add the ammoniacal liquor adjust pH to 8-8.5, discharging.
Embodiment 3
Preparation water-based ink raw materials used consumption during with synthetic resins: 190 kilograms, turps, 330 kilograms of butyl acrylates, 80 kilograms of vinylbenzene, 330 kilograms of vinyl-acetic esters, 30 kilograms of methacrylic acids, 40 kilograms of tertiary ethylene carbonates (Dutch shell), 5.2 kilograms of Potassium Persulphates, catalyzer: 4.8 kilograms, the mixture of Benzyl Chloride and aluminum chloride (mass ratio is 1:1).
Water-based ink is as follows with the concrete preparation process of synthetic resins:
1. terpenes prepolymer preparation
[1] catalyzer is added in the mixed solvent that is formed by 36kg ethyl acetate and 4kg toluene mixing;
[2] drop into reactor with turps with by the mixed solvent that 144kg ethyl acetate and 16kg toluene form, stir;
[3] when temperature of reaction kettle reaches 10 ℃, the catalyst solution of step [1] gained is added in reactor, keep temperature of reaction kettle and be no more than 15 ℃, reacted 3 hours;
[4] 200kg hot water (temperature is 80 ℃) is added reactor carry out the hot water hydrolysis, stir after 10 minutes, solids removed by filtration impurity, the filtrate standing demix, get organic phase and with hot water wash to neutral Zai＜=0.015MPa, temperature is that under 75-85 ℃, decompression steams organic solvent and residual reactant, obtains the terpenes prepolymer;
[5] 900kg water, emulsifying agent 6.5kg (OP-10 is 2:1 with the mass ratio of Sodium dodecylbenzene sulfonate) are mixed with the terpenes prepolymer, stirring is warming up to 50 ℃ of emulsifications and obtains the terpenes pre-polymer emulsion, and is standby;
[6] with the initiator (Potassium Persulphate) of 100kg water and 5.2kg, add in dissolving vessel, be stirred to dissolving fully, obtain initiator solution;
[7] butyl acrylate, vinylbenzene, vinyl-acetic ester, methacrylic acid and tertiary ethylene carbonate are mixed, obtain monomer mixture;
[8] first 1/3 monomer mixture of measuring is added in the terpenes pre-polymer emulsion, stirring and evenly mixing, when being warming up to 60 ℃ under agitation condition, the monomer mixture of the amount of 2/3 under remaining with 1.5～2 hours again and the initiator solution of 2/3 amount splash into, and monomer mixture and initiator solution are synchronously dripped off, be incubated after 10 minutes, splash into the initiator solution of remaining 1/3 amount, dripped off with 20-30 minute, below temperature-stable to 80 ℃, be warming up to 90-95 ℃ after dripping, insulation 30min, vacuumize (＜=0.015MPa) and remove the complete monomer of unreacted, cooling, add the ammoniacal liquor adjust pH to 8-8.5, discharging.
Claims (10)
1. the preparation method of a water-based ink use synthetic resins, is characterized in that, comprises the steps:
(1) turps is dissolved in organic solvent, then adds catalyzer to react under 5～15 ℃ 1～5 hour, described catalyzer is the mixture of Benzyl Chloride and aluminum chloride;
(2) add water in the reaction solution of step (1), stir, filter, the filtrate standing demix obtains organic layer, and organic layer washes with water to neutrality, then steaming obtains the terpenes prepolymer except organic solvent;
(3) terpenes prepolymer and emulsifying agent are added to the water, heated and stirred is made the terpenes pre-polymer emulsion;
(4) butyl acrylate, methyl methacrylate, vinyl-acetic ester and active function groups monomer are mixed to get monomer mixture;
(5) being added in the terpenes pre-polymer emulsion the first part of monomer mixture, after heated and stirred is even, under 60～80 ℃, partly initiator and remaining monomer mixture are added again, react after 10～20 minutes, again remaining initiator is added, then be warming up to 90～95 ℃ of reactions 20～40 minutes, cooling.
2. preparation method according to claim 1 is characterized in that: described catalyzer by Benzyl Chloride and aluminum chloride by weight being 1:(0.5～2) form.
3. preparation method according to claim 1 and 2, it is characterized in that: the consumption of described catalyzer is 2.5～7.5% of turps weight.
4. preparation method according to claim 1, it is characterized in that: described emulsifying agent is the mixture of OP-10 and Sodium dodecylbenzene sulfonate.
5. preparation method according to claim 1, it is characterized in that: count by weight, the consumption of raw material is as follows: 15～21 parts, turps, 15～45 parts of butyl acrylates, 7～15 parts of methyl methacrylates, 20～35 parts of vinyl-acetic esters, 6～12 parts of active function groups monomers, 0.35～0.6 part of initiator.
6. preparation method according to claim 1 or 5, it is characterized in that: described initiator is persulphate.
7. preparation method according to claim 1 or 5 is characterized in that: described active function groups monomer is at least a in vinylformic acid, methacrylic acid, Hydroxyethyl acrylate, Propylene glycol monoacrylate, tertiary ethylene carbonate and glycidyl acrylate.
8. preparation method according to claim 1 or 5, it is characterized in that: described methyl methacrylate replaces with vinylbenzene.
9. water-based ink synthetic resins, it is characterized in that: described water-based ink synthetic resins is to make according to the arbitrary described method of claim 1～9.
10. the application of the described synthetic resins of claim 9 is characterized in that: the application of described synthetic resins in preparation plastics aquosity intaglio printing ink.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013100599348A CN103122050A (en) | 2013-02-26 | 2013-02-26 | Synthetic resin for water-soluble printing ink and preparation method thereof |
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| CN2013100599348A CN103122050A (en) | 2013-02-26 | 2013-02-26 | Synthetic resin for water-soluble printing ink and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892821A (en) * | 2015-05-27 | 2015-09-09 | 合肥卓元科技服务有限公司 | Preparation method of vinyl acetate-vinyl versatate copolymer emulsion |
| CN105273494A (en) * | 2015-11-27 | 2016-01-27 | 重庆宏元油墨有限责任公司 | Waterborne printing ink for non-woven fabric and preparation method of waterborne printing ink |
| CN106046235A (en) * | 2016-06-27 | 2016-10-26 | 合众（佛山）化工有限公司 | Water-based ink resin binder and preparation method thereof |
| CN107266623A (en) * | 2017-07-25 | 2017-10-20 | 杭州海维特化工科技有限公司 | A kind of PVC floor film water inkwood fat and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709927A (en) * | 2005-07-08 | 2005-12-21 | 广西大学 | Method for preparing colorless terpene resin |
-
2013
- 2013-02-26 CN CN2013100599348A patent/CN103122050A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709927A (en) * | 2005-07-08 | 2005-12-21 | 广西大学 | Method for preparing colorless terpene resin |
Non-Patent Citations (3)
| Title |
|---|
| 吴喜来等: "含萜烯树脂丙烯酸酯乳液型压敏胶的制备与性能研究", 《中国胶粘剂》, vol. 21, no. 8, 31 August 2012 (2012-08-31) * |
| 夏宇正等: "增粘树脂与丙烯酸酯共存下的乳液聚合行为", 《北京化工大学学报》, vol. 34, 31 December 2007 (2007-12-31), pages 44 - 47 * |
| 胡树文等: "溶有增粘树脂的丙烯酸酯乳液共聚及压敏胶的性能", 《高分子学报》, no. 6, 31 December 1997 (1997-12-31), pages 709 - 714 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892821A (en) * | 2015-05-27 | 2015-09-09 | 合肥卓元科技服务有限公司 | Preparation method of vinyl acetate-vinyl versatate copolymer emulsion |
| CN105273494A (en) * | 2015-11-27 | 2016-01-27 | 重庆宏元油墨有限责任公司 | Waterborne printing ink for non-woven fabric and preparation method of waterborne printing ink |
| CN106046235A (en) * | 2016-06-27 | 2016-10-26 | 合众（佛山）化工有限公司 | Water-based ink resin binder and preparation method thereof |
| CN107266623A (en) * | 2017-07-25 | 2017-10-20 | 杭州海维特化工科技有限公司 | A kind of PVC floor film water inkwood fat and preparation method thereof |
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