CN104559794B - Preparation method of alcohol soluble acrylic rosin resin - Google Patents
Preparation method of alcohol soluble acrylic rosin resin Download PDFInfo
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- CN104559794B CN104559794B CN201310685995.5A CN201310685995A CN104559794B CN 104559794 B CN104559794 B CN 104559794B CN 201310685995 A CN201310685995 A CN 201310685995A CN 104559794 B CN104559794 B CN 104559794B
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Abstract
The invention discloses a preparation method of alcohol soluble acrylic rosin resin and belongs to the technical field of rosin processing. The preparation method comprises the following steps: by taking rosin as a raw material, modifying by using acrylic acid; then, carrying out esterification reaction with glycerinum to obtain the alcohol soluble acrylic rosin resin. The prepared product alcohol soluble acrylic rosin resin has excellent performances of light color, high softening point, rapid dryness and good alcohol solubility, can satisfy the using requirement of environment-friendly water-based printing ink and alcohol soluble plate printing ink and is suitable for alcohol soluble and water-based products such as water-based coatings, oil polish and the like, and use of toxic organic solvents such as methylbenzene, dimethylbenzene, ethyl acetate and the like can be avoided.
Description
Technical field
The invention belongs to Colophonium processing technique field, especially a kind of preparation method of alcohol-soluble acrylic acid rosin resin.
Background technology
Traditional oil-based ink is using organic solvent such as toluene, dimethylbenzene, ethyl acetate, ethers, ketone etc. as auxiliary agent
, 40%～60% is up to containing organic solvent in obtained ink, it is dried by volatilization when using, cause printing cost high.Have
The characteristics of machine solvent toluene, dimethylbenzene, ethyl acetate and alcohols, ethers, ketone typically have volatile, inflammable, what is used
During pole fire hazardous and blast danger；Further, since these organic solvents are poisonous, volatile, so can be dirty
The manufacture of dye ink and the environment of printing, endanger the healthy of shop worker, while manufacture in ink being discharged with the process of printing
Tail gas or waste water also can the local water resource environment of pollutant atmosphere and destruction；And, during package printed matter, have
Some poisonous and harmful substances of machine solvent type ink can be remained in leaflet, so as to polluting, endangering, particularly when
Used in the strict packages printing of the hygienic requirements such as cigarette, wine, food, medicine, beverage, toy for children if this kind of ink, cause
Consequence will be more serious.With the development in epoch, various new products and new technique emerge in an endless stream, and entire society's environmental consciousness is increasingly
Strengthen, people adhesive, the package printed matter closely bound up to daily life etc. are extremely paid close attention to, traditional ink etc. is containing poisonous residual
Staying the product of material will be limited and be forbidden.
And Colophonium and its modified deep processed product can be used as producing the primary raw material of resin for printing ink, its production is obtained
Ink resin have good wetting effect to pigment, with gel appropriate reaction after can obtain the company with certain viscoelasticity
Ramming material, thus be widely used in printing-ink.
The content of the invention
The present invention provides a kind of preparation method of alcohol-soluble acrylic acid rosin resin, its obtained alcohol-soluble acrylic resin
Environment-friendly type aqueous ink, the use requirement of alcohol-soluble gravure printing ink can be met, and suitable for water paint and oil polish etc.
In alcohol-soluble and aqueous product, can avoid using the toxic organic solvents such as toluene, dimethylbenzene, ethyl acetate.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of alcohol-soluble acrylic acid rosin resin is comprised the following steps：
A. first Colophonium is put in reactor and is heated, when the Colophonium temperature of charge reaches 150 DEG C～160 DEG C,
Reactor agitator is started, 4,4`- thiobiss are then added in the reactor（The 6- tert-butyl group -3- methylphenols）Carry out anti-
Should, and continue heating；
B. when the material in reactor temperature reaches 195 DEG C～200 DEG C, acrylic acid is added in the reactor,
And closed reactor, then react 2 hours in the case where the reactor pressure is 0.1 MPa～0.3 MPa；
C. when described in step B reaction terminate after, by the reactor release emptying, add glycerol, and be heated to 250 DEG C～
255 DEG C carry out esterification 1 hour；
D. after reaction terminates described in step C, vacuum pump is opened to carrying out evacuation 0.5 hour in the reactor, so
After start cooling；When temperature is down to 200 DEG C, the material that reaction is obtained removes impurity with 200 mesh sock filtrations, that is, obtain this
Alcohol-soluble acrylic acid rosin resin；
Wherein, the Colophonium, 4,4`- thiobiss（The 6- tert-butyl group -3- methylphenols）, the mass ratio of acrylic acid and glycerol is
100：0.1：7.5：4.2.
In above-mentioned technical proposal, more specifically technical scheme is in the preparation process, in reactor nitrogen to be passed through
As protective gas.
Due to adopting above-mentioned technical proposal, the beneficial effect that the present invention is obtained to be：
1. the present invention is, with Colophonium as raw material, to be modified using acrylic acid, then carries out esterification with glycerol, obtains alcohol
Soluble acrylic rosin resin, obtained product alcohol-soluble acrylic acid rosin resin has of light color, softening point high, quick-drying and very
The premium properties of good alcohol-soluble, can meet the use requirement in environment-friendly type aqueous ink, alcohol-soluble gravure printing ink, and fit
In for alcohol-solubles and aqueous product such as water paint and oil polishes, can avoid having using toluene, dimethylbenzene, ethyl acetate etc.
Malicious organic solvent.
2. the alcohol-soluble acrylic acid rosin resin for being prepared by the present invention is used in the production of alcohol-soluble gravure printing ink, danger
Evil is very little, produces the alcohol-soluble gravure printing ink that obtains and can be applicable to food, medicine, beverage, tobacco and wine and with human contact's
The aspects such as articles for daily use packages printing.Alcohol-soluble gravure printing ink can solve the problem that the benzene injury that toluene class ink is caused to health
With the problem of benzene remaining influence packaging quality so that its competitiveness on plastic flexible package print field is greatly improved.
Specific embodiment
Below in conjunction with example, the invention will be further described：
A kind of preparation method of alcohol-soluble acrylic acid rosin resin is comprised the following steps：
A. first 210Kg Colophonium is put in reactor and is heated, when the Colophonium temperature of charge reaches 150 DEG C～160
DEG C when, start reactor agitator, 0.21Kg4,4`- thiobiss are then added in the reactor（The 6- tert-butyl group -3- methyl
Phenol）Reacted, and continued heating；
B. when the material in reactor temperature reaches 195 DEG C～200 DEG C, 15.8Kg third is added in the reactor
Olefin(e) acid, and closed reactor, then react 2 hours in the case where the reactor pressure is 0.1 MPa～0.3 MPa；
C. after reaction terminates described in step B, by reactor release emptying, 8.8Kg glycerol is added, and is heated to
250 DEG C～255 DEG C carry out esterification 1 hour；
D. after reaction terminates described in step C, vacuum pump is opened to carrying out evacuation 0.5 hour in the reactor, so
After start cooling；When temperature is down to 200 DEG C, the material that reaction is obtained removes impurity with 200 mesh sock filtrations, that is, obtain this
Alcohol-soluble acrylic acid rosin resin；
Alcohol-soluble acrylic acid rosin resin obtained in the present invention is carried out into product quality detection, the result for obtaining such as table 1.
Table 1
Claims (2)
1. a kind of preparation method of alcohol-soluble acrylic acid rosin resin, it is characterised in that comprise the following steps：
A. first Colophonium is put in reactor and is heated, when the Colophonium temperature of charge reaches 150 DEG C～160 DEG C, started
Reactor agitator, then adds 4,4`- thiobiss in the reactor（The 6- tert-butyl group -3- methylphenols）Reacted,
And continue to heat；
B. when the material in reactor temperature reaches 195 DEG C～200 DEG C, acrylic acid is added in the reactor, and it is close
Reactor is closed, is then reacted 2 hours in the case where the reactor pressure is 0.1 MPa～0.3 MPa；
C. after reaction terminates described in step B, by reactor release emptying, glycerol is added, and is heated to 250 DEG C～255
DEG C carry out esterification 1 hour；
D. after reaction terminates described in step C, vacuum pump is opened to carrying out evacuation 0.5 hour in the reactor, Ran Houkai
Begin to lower the temperature；When temperature is down to 200 DEG C, the material that reaction is obtained removes impurity with 200 mesh sock filtrations, that is, obtain this alcohol molten
Property acrylic acid rosin resin；
Wherein, the Colophonium, 4,4`- thiobiss（The 6- tert-butyl group -3- methylphenols）, the mass ratio of acrylic acid and glycerol is 100：
0.1：7.5：4.2.
2. a kind of preparation method of alcohol-soluble acrylic acid rosin resin according to claim 1, it is characterised in that the system
During standby, nitrogen is passed through in reactor as protective gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310685995.5A CN104559794B (en) | 2013-12-16 | 2013-12-16 | Preparation method of alcohol soluble acrylic rosin resin |
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| CN201310685995.5A CN104559794B (en) | 2013-12-16 | 2013-12-16 | Preparation method of alcohol soluble acrylic rosin resin |
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| CN104559794A CN104559794A (en) | 2015-04-29 |
| CN104559794B true CN104559794B (en) | 2017-05-10 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105778767A (en) * | 2016-04-15 | 2016-07-20 | 梧州市飞卓林产品实业有限公司 | Method for preparing alcohol-soluble rosin resin |
| CN106519986B (en) * | 2016-09-23 | 2019-05-28 | 广东科茂林产化工股份有限公司 | A kind of tackifying resin and preparation method thereof prepared by retinal regenerant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768240A (en) * | 2010-01-26 | 2010-07-07 | 广西民族大学 | Abietyl-containing terpolymer and preparation method thereof |
| CN102965022A (en) * | 2012-12-04 | 2013-03-13 | 李先兰 | Preparation method of acrylic modified rosin glyceride resin |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103517957B (en) * | 2011-04-11 | 2015-06-10 | 阿利桑那化学公司 | Rosin esters for non-wovens |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768240A (en) * | 2010-01-26 | 2010-07-07 | 广西民族大学 | Abietyl-containing terpolymer and preparation method thereof |
| CN102965022A (en) * | 2012-12-04 | 2013-03-13 | 李先兰 | Preparation method of acrylic modified rosin glyceride resin |
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