CN103205155B - Method for preparing printing ink thickener - Google Patents
Method for preparing printing ink thickener Download PDFInfo
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- CN103205155B CN103205155B CN201310154488.9A CN201310154488A CN103205155B CN 103205155 B CN103205155 B CN 103205155B CN 201310154488 A CN201310154488 A CN 201310154488A CN 103205155 B CN103205155 B CN 103205155B
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Abstract
The invention discloses a method for preparing a printing ink thickener. The method comprises the following steps of: dissolving aluminum isopropoxide into an organic solvent, stirring and heating to 80-130 DEG C, dropwise adding an organic acid to the heated solution of aluminum isopropoxide and the organic solvent; heating to 140-190 DEG C, adding water to carry out hydrolysis reaction after heating for a period of time; at the end of the hydrolysis reaction, adding the organic solvent for aging and cooling, and filtering; and adding water to remove insoluble substances in the reaction system to obtain the organic solution with certain aluminum content. The preparation method of the printing ink thickener does not need pre-diluting; the materials are added at a high temperature; the prepared product does not generate organic matters such as alcohols in the using process; the preparation method is simple; and the thickening effect is significant.
Description
Technical field
The present invention relates to the compounding process field of ink thickening material, be specifically related to a kind of preparation method of liquid ink thickening material.
Background technology
Thickening material is very important auxiliary agent during flexographic ink is produced, and is the key component that ink is manufactured binder, improves the rheological of ink by changing the viscosity of binder, and then improves the ability that ink adapts to high speed printing.The thickening material that at present flexographic ink is used is generally organo-aluminium compound, in binder preparation process, add, under certain temperature condition with wherein resin, vegetables oil in hydroxyl or carboxyl generation crosslinking reaction, thereby increase viscosity.But existing thickening material in use needs to dilute in advance with solvent, and can not at high temperature carry out, system temperature need to be down to 150 ℃ adds thickening material to be uniformly dispersed below, and then be warming up to more than 170 ℃, otherwise directly add membership in the time of 170 ℃, to produce local thickening excessive, and silly line particle affects ink performance.Produce and consuming timely waste energy again, in addition, the alcohol type organic producing in thickening reaction process pollutes the environment.
Summary of the invention
The object of the invention is to: for the deficiencies in the prior art, the invention provides and a kind ofly without pre-dilution, goods, can under more than 170 ℃ high temperature, directly add and carry out thickening reaction and product in use without the preparation method of the ink thickening material of alcohol type organic generation, preparation method is simple, and thickening effectiveness is obvious and environment friendly and pollution-free.
To achieve these goals, the present invention has adopted following technical scheme:
A kind of preparation method of ink thickening material, comprise the following steps: by aluminum isopropylate and organic solvent according to weight ratio 1:(0.2-0.5) mix, stir and heat up 0.5-1h to 80-130 ℃, then in 1-1.5h, in the solution after both heating, drip the 2 ethyl hexanoic acid with aluminum isopropylate equimolar amount, carry out replacement(metathesis)reaction, after replacement(metathesis)reaction finishes, reheat to 140-190 ℃, add the water reaction that is hydrolyzed, after hydrolysis reaction finishes, add organic solvent fast cooling, when reaching 50-70 ℃, temperature filters, remove by filter the insolubles in reaction system, obtain the organic solution that aluminium content is 7-9%.
As preferably, described organic solvent is one or both in mineral oil, 2 ethyl hexanoic acid-1-methyl ethyl ester, 88 ℃ of the aniline point > of described mineral oil.Adopt after above-mentioned preferred version, aniline point can occasionally strengthen the thickening effectiveness of thickening material at more than 88 ℃ mineral oil, and has more general adaptability, and 2 ethyl hexanoic acid-1-methyl ethyl ester has good solubility to ink.
As preferably, the described mode that adds water is that alcohol water adds or ties crystal water and adds.Adopt after above-mentioned preferred version, adopt the above-mentioned water feeding method can controlled hydrolysis speed of reaction.
As preferably, described water and the mol ratio of aluminum isopropylate are (0.5-1.5): 1.Adopt after above-mentioned preferred version, if water and aluminum isopropylate mol ratio lower than 0.5, hydrolysis reaction will be not exclusively; And if water and aluminum isopropylate mol ratio are greater than 1.5, can produce the harmful side products such as dihydroxyl aluminium.
As preferably, described aluminum isopropylate and the mass ratio of solvent are 1:(0.5-1).Adopt after above-mentioned preferred version, the thickening material that the aluminum isopropylate of above-mentioned mass ratio and solvent make has good mobility.
As preferably, described aluminum isopropylate and organic solvent are according to weight ratio 1:(0.2-0.5) mix after, stir and heat up 0.5-1h to 80-90 ℃.Adopt after above-mentioned preferred version,
As preferably, described replacement(metathesis)reaction finishes post-heating 1-2h.Adopt after above-mentioned preferred version, can guarantee that 2 ethyl hexanoic acid all participates in reaction.
As preferably, the time of described hydrolysis reaction is 3-5h.Adopt after above-mentioned preferred version, the time of hydrolysis reaction is more reasonable, effectively controlled hydrolysis speed of response.
As preferably, described filter method is millipore filtration.Adopt after above-mentioned preferred version, filter effect is better, can remove insolubles, improves the clarity of liquid.
2 ethyl hexanoic acid in the preparation method of ink thickening material of the present invention is with branched structure, under normal temperature, be liquid, easy to use, there is satisfactory stability and water resisting property, after hydrolysis reaction finishes, adding organic solvent to carry out fast cooling can avoid the long color and luster causing of high-temperature residence time to change, the ink thickening material that utilizes method of the present invention to prepare, in use without pre-dilution, and can at high temperature add, the product making produces without organism such as alcohols in thickening, preparation method is simple, and thickening effectiveness is obvious.
Embodiment
embodiment 1
Load weighted aluminum isopropylate 204g and mineral oil 65g are joined in the 1000ml four-hole boiling flask with condensing works, stir, be heated to 80 ℃, drip 144g2-thylhexoic acid and carry out replacement(metathesis)reaction, reaction times is 1h, after replacement(metathesis)reaction finishes, reheat 1h and be warming up to 140 ℃, the Virahol 150g that to drip water content be 12% reaction that is hydrolyzed, hydrolysis time is 5h, then add 65g mineral oil fast cooling to 60 ℃, through filtering, to obtain aluminium content be 8.5% clarification pale yellow oily liquid body 316 g.
Resin, oleum lini, kerosene are warming up to 210 ℃ according to the ratio mix and blend of weight ratio 2:1:2, are incubated 15 minutes, then naturally cool to 25 ℃, make sylvic oil, viscosity is 35Pa.s.Get 100g sylvic oil, be warming up to 170 ℃, add above prepared thickening material 1.48 g, after dispersed with stirring is even, be warming up to 175 ℃, be incubated 30 minutes, be naturally cooled to 25 ℃, test its viscosity, sylvic oil viscosity is increased to 130Pa.s.
embodiment 2
The aluminum isopropylate 102g measuring and mineral oil 50g are joined in the 1000ml four-hole boiling flask with condenser, stir, be heated to 95 ℃, drip 72g2-thylhexoic acid and carry out replacement(metathesis)reaction, reaction times is 1h, after replacement(metathesis)reaction finishes, reheat and be warming up to 190 ℃, adding water-content is 45.7% crystalline sulfuric acid aluminium 14.2g, reaction is hydrolyzed, hydrolysis time is 3h, then adds 25g mineral oil fast cooling to 60 ℃, and through filtering, to obtain aluminium content be 8.18% clarification pale yellow oily liquid body 165g.
By above prepared thickening material 1.54g, be added in the prepared sylvic oil of 100g " embodiment 1 ", be warming up to 170 ℃, after dispersed with stirring is even, be warming up to 175 ℃, be incubated 30 minutes, be naturally cooled to 25 ℃, test its viscosity, sylvic oil viscosity is increased to 136Pa.s.
embodiment 3
The aluminum isopropylate 204g measuring and 2 ethyl hexanoic acid-1-methyl ethyl ester 50g are joined in the 1000ml four-hole boiling flask with condenser, stir, be heated to 85 ℃, drip 144g2-thylhexoic acid and carry out replacement(metathesis)reaction, reaction times is 1.5h, after replacement(metathesis)reaction finishes, reheat and be warming up to 190 ℃, adding water-content is 45.7% crystalline sulfuric acid aluminium 28g, reaction 4h is hydrolyzed, after hydrolysis reaction finishes, add 2 ethyl hexanoic acid-1-methyl ethyl ester 101g, cool to 60 ℃ and filter, obtain aluminium content and be 8.03% clarification pale yellow oily liquid body 336 g.
By above prepared gelifying agent 1.58 g, be added in the prepared sylvic oil of 100g " embodiment 1 ", be warming up to 175 ℃, dispersed with stirring is evenly rear is incubated 30 minutes, is then naturally cooled to 25 ℃, tests its viscosity, and sylvic oil viscosity is increased to 121Pa.s.
embodiment 4
The aluminum isopropylate 204g measuring and mineral oil 50g are joined in the 1000ml four-hole boiling flask with condenser, stir, heating 0.5h is warming up to 85 ℃, drip 144g isocaprylic acid and carry out replacement(metathesis)reaction, reaction times is 1h, after replacement(metathesis)reaction finishes, reheat and be warming up to 190 ℃, the Virahol 90g that to drip water content be 30% reaction that is hydrolyzed, hydrolysis time is 5h, then add 2 ethyl hexanoic acid-1-methyl ethyl ester 114g to cool to 60 ℃, through filtering, to obtain aluminium content be 7.71% clarification pale yellow oily liquid body 350g.
By above prepared gelifying agent 1.63g, be added in the prepared sylvic oil of 100g " embodiment 1 ", be warming up to 175 ℃, dispersed with stirring is evenly rear is incubated 30 minutes, is then naturally cooled to 25 ℃, tests its viscosity, and sylvic oil viscosity is increased to 124Pa.s.
embodiment 5
The aluminum isopropylate 204g measuring and 2 ethyl hexanoic acid-1-methyl ethyl ester 40.8g are joined in the 1000ml four-hole boiling flask with condenser, stir, be heated to 83 ℃, drip 144g isocaprylic acid and carry out replacement(metathesis)reaction, reaction times is 1.5h, after replacement(metathesis)reaction finishes, reheat and be warming up to 140 ℃, Virahol 150 g that to drip water content be 12% reaction that is hydrolyzed, polymerization reaction time is 5h, then add mineral oil 73g to cool to 60 ℃, through filtering, to obtain aluminium content be 9.0% clarification pale yellow oily liquid body 300g.
By above prepared gelifying agent 1.4g, be added in the prepared sylvic oil of 100g " embodiment 1 ", be warming up to 175 ℃, dispersed with stirring is evenly rear is incubated 30 minutes, is then naturally cooled to 25 ℃, tests its viscosity, and sylvic oil viscosity is increased to 128Pa.s.
embodiment 6
The aluminum isopropylate 250kg measuring and mineral oil 125kg are joined in the reactor with condenser, stir, heat and within 45 minutes, be warming up to 85 ℃, drip 176.5 kg isocaprylic acids and carry out replacement(metathesis)reaction, reaction times is 1.5h, after replacement(metathesis)reaction finishes, reheat and be warming up to 155 ℃, adding water-content is the Virahol 73kg of 30 %, reaction is hydrolyzed, hydrolysis time is 5h, then adds mineral oil 119kg to cool to 60 ℃, and through filtering, to obtain aluminium content be 7.0% clarification pale yellow oily liquid body 472kg.
By above prepared thickening material 1.80g, be added in the prepared sylvic oil of 100g " embodiment 1 ", after dispersed with stirring is even, be warming up to 175 ℃, be incubated 30 minutes, be naturally cooled to 25 ℃, test its viscosity, sylvic oil viscosity is increased to 136Pa.s.
Claims (7)
1. the preparation method of an ink thickening material, it is characterized in that comprising the following steps: by aluminum isopropylate and organic solvent according to weight ratio 1:(0.2-0.5) mix, stir and heat up 0.5-1h to 80-130 ℃, then in 1-1.5h, in the solution after both heating, drip the 2 ethyl hexanoic acid with aluminum isopropylate equimolar amount, carry out replacement(metathesis)reaction, after replacement(metathesis)reaction finishes, reheat to 140-190 ℃, add the water reaction that is hydrolyzed, after hydrolysis reaction finishes, add organic solvent fast cooling, when reaching 50-70 ℃, temperature filters, remove by filter the insolubles in reaction system, obtain the organic solution that aluminium content is 7-9%, described organic solvent is one or both in mineral oil, 2 ethyl hexanoic acid-1-methyl ethyl ester, 88 ℃ of the aniline point > of described mineral oil.
2. the preparation method of ink thickening material according to claim 1, is characterized in that: the described mode that adds water is that alcohol water adds or ties crystal water and adds.
3. the preparation method of ink thickening material according to claim 1, is characterized in that: described water and the mol ratio of aluminum isopropylate are (0.5-1.5): 1.
4. the preparation method of ink thickening material according to claim 1, is characterized in that: described aluminum isopropylate and organic solvent are according to weight ratio 1:(0.2-0.5) mix after, stir and heat up 0.5-1h to 80-90 ℃.
5. the preparation method of ink thickening material according to claim 1, is characterized in that: described replacement(metathesis)reaction finishes post-heating 1-2h.
6. the preparation method of ink thickening material according to claim 1, is characterized in that: the time of described hydrolysis reaction is 3-5h.
7. the preparation method of ink thickening material according to claim 1, is characterized in that: described filter method is millipore filtration.
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| CN103205155B true CN103205155B (en) | 2014-12-03 |
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| CN103740168A (en) * | 2013-12-14 | 2014-04-23 | 常熟市淼泉盛达助剂厂 | Preparation method of printing ink thickening agent |
| CN104211968B (en) * | 2014-09-17 | 2017-01-25 | 浙江省中明化工科技有限公司 | Preparation process for preparing mineral oil-based aluminum-oxygen polymer by using dihydroxyl aluminum carboxylate intermediate |
| CN107936684A (en) * | 2017-11-03 | 2018-04-20 | 安徽九天印务有限公司 | A kind of plastic printing ink concentration thickening process |
| CN111035787A (en) * | 2019-12-31 | 2020-04-21 | 江门市和馨香精技术有限公司 | Fragrance and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0952463A (en) * | 1995-08-10 | 1997-02-25 | Riso Kagaku Corp | Fixing method of printing water base ink and water base ink |
| CN101456569A (en) * | 2008-07-22 | 2009-06-17 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for quick-speed preparing aerogel by hydro-thermal synthesis at low cost |
| CN101712614A (en) * | 2008-10-06 | 2010-05-26 | 天津市化学试剂研究所 | Method for preparing 2-ethyl hexahydric aluminum |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3958325B2 (en) * | 2004-03-16 | 2007-08-15 | キヤノン株式会社 | Print medium coating liquid, ink jet ink, image forming method, set of print medium coating liquid and ink jet ink, and ink jet recording apparatus |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0952463A (en) * | 1995-08-10 | 1997-02-25 | Riso Kagaku Corp | Fixing method of printing water base ink and water base ink |
| CN101456569A (en) * | 2008-07-22 | 2009-06-17 | 绍兴纳诺气凝胶新材料研发中心有限公司 | Method for quick-speed preparing aerogel by hydro-thermal synthesis at low cost |
| CN101712614A (en) * | 2008-10-06 | 2010-05-26 | 天津市化学试剂研究所 | Method for preparing 2-ethyl hexahydric aluminum |
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Inventor after: Li Qichun Inventor after: Wu Zushen Inventor after: Weng Qifei Inventor after: Dai Pinzhong Inventor after: Zhou Ruochen Inventor before: Li Qichun Inventor before: Wu Zusang Inventor before: Weng Qifei Inventor before: Dai Pinzhong Inventor before: Zhou Ruochen |
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Free format text: CORRECT: INVENTOR; FROM: LI QICHUN WU ZUSANG WENG QIFEI DAI PINZHONG ZHOU RUOCHEN TO: LI QICHUN WU ZUSHEN WENG QIFEI DAI PINZHONG ZHOU RUOCHEN |