CN105566548B - Resin and its chemical synthesis process used in a kind of correction fluid and a kind of correction fluid - Google Patents
Resin and its chemical synthesis process used in a kind of correction fluid and a kind of correction fluid Download PDFInfo
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- CN105566548B CN105566548B CN201610071257.5A CN201610071257A CN105566548B CN 105566548 B CN105566548 B CN 105566548B CN 201610071257 A CN201610071257 A CN 201610071257A CN 105566548 B CN105566548 B CN 105566548B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D10/00—Correcting fluids, e.g. fluid media for correction of typographical errors by coating
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention provides a kind of chemical synthesis process of resin used in correction fluid, resin used in a kind of correction fluid and a kind of correction fluid, the method is with methyl methacrylate, butyl acrylate, it is two or more as soft monomer in Isooctyl acrylate monomer and hydroxy-ethyl acrylate, styrene is as hard monomer, azodiisobutyronitrile is catalyst, hexamethylene is solvent, it is heated to reflux by soft monomer, hard monomer, first mix monomer of catalysts and solvents composition, reaction the first mixed liquor of generation, the second mix monomer being made of soft monomer and hard monomer is slowly added dropwise into the first mixed liquor, the second mixed liquor is obtained by the reaction, azodiisobutyronitrile is added in into the second mixed liquor, resin used in correction fluid is obtained by the reaction.The method of the embodiment of the present invention is prepared for resin used in the correction fluid with preferable caking property and dispersiveness by the usage ratio for controlling various reaction reagents and specific reaction condition；Simultaneously using the method that monomer is added portionwise, it ensure that reacting balance carries out.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of chemical synthesis process of resin used in correction fluid, one
Resin and a kind of correction fluid used in kind correction fluid.
Background technology
China is to invent earliest in the world and the country using correction fluid.When early Medieval China, people have just started
It covers using correction fluid, correct the mistake among writing.Until nineteen fifty-one American's BETTY BOOP Naismith Lindsey Graham
Correction fluid is invented.
Correction fluid also known as " opaquing fluid ", " correcting fluid " are contemporary work, the common common stationery of study.A kind of high quality
Correction liquid energy make one easily modify article or file work, and original form of file can be kept, after modification
The trace that also can't see modification is duplicated again, is brought great convenience to the working and learning of people.
Modern correction fluid is mainly made of three parts：That is covering agent, link stuff and adjuvant.Wherein, covering agent plays covering
Effect；Link stuff is made of film forming matter and solvent, and film forming matter plays adherency, scattered covering agent, and solvent makes film forming matter
Matter dissolving disperses, and volatilizees rapidly, dries after use；Auxiliary agent, i.e. certain distinctive application performance of imparting correction fluid are added auxiliary
Chemicals is helped, such as adding in essence can make correction fluid have certain fragrance.
There is common correction fluid hardness not reach requirement, it is dry after row pen is not smooth when being write on coating, drag
Phenomenon places the defects of lamination occur for a long time.Therefore, it is badly in need of a kind of preferable hardness, row pen smoothness, nothing and drags a phenomenon
Not stratified high-performance correction fluid is placed for a long time.
The content of the invention
The present invention provides the chemical synthesis process of resin used in a kind of correction fluid, resin and one kind used in a kind of correction fluid
Correction fluid solves above-mentioned technical problem with all or part of.
The invention discloses a kind of chemical synthesis process of resin used in correction fluid, comprise the following steps：
Step (1), with two in methyl methacrylate, butyl acrylate, Isooctyl acrylate monomer and hydroxy-ethyl acrylate
Kind or more as soft monomer, for styrene as hard monomer, azodiisobutyronitrile is catalyst, and hexamethylene is solvent, is heated to reflux
The first mix monomer being made of the soft monomer, the hard monomer, the catalyst and the solvent reacts 1~2h, generation
First mixed liquor,
In first mix monomer, the methyl methacrylate and the mass ratio of the styrene stated is 0.117
~0.162, the mass ratio of the butyl acrylate and the styrene is 0.157~0.244, the hydroxy-ethyl acrylate and institute
The mass ratio of styrene is stated as 0.08~0.139, the mass ratio of the Isooctyl acrylate monomer and the styrene for 0.591~
0.75, the mass ratio of the azodiisobutyronitrile and the styrene is 0.014~0.031, the hexamethylene and the benzene second
The mass ratio of alkene is 1.909~2.778；
Second be made of the soft monomer and the hard monomer is slowly added dropwise into first mixed liquor for step (2)
Mix monomer is added dropwise in 2~4h, obtains the second mixed liquor,
In second mix monomer, the mass ratio for stating methyl methacrylate and the styrene for 0.1~
0.148, the mass ratio of the butyl acrylate and the styrene is 0.143~0.222, the hydroxy-ethyl acrylate with it is described
The mass ratio of styrene is 0.074~0.11, the mass ratio of the Isooctyl acrylate monomer and the styrene for 0.524~
0.654；
Step (3) adds in azodiisobutyronitrile into second mixed liquor, and flow back 3~4h, after reaction, cooling
To 30~40 DEG C of dischargings, resin used in the correction fluid is obtained, wherein the azodiisobutyronitrile and institute in the step (3)
The mass ratio for stating the styrene in step (2) is 0.01~0.022.
Optionally, first mix monomer is identical with the monomeric species contained by second mix monomer.
Optionally, resin used in the correction fluid is prepared by the above method；
Resin used in the correction fluid has viscosity and dispersiveness.
Optionally, the resin included in the correction fluid is resin used in the correction fluid prepared by the above method；
After coating is dry, coating will not rupture the correction fluid because of writing, be not in drag a phenomenon；
The correction fluid is placed for a long time to be occurred without lamination.
Compared with prior art, the present invention includes advantages below：
The present invention provides a kind of chemical synthesis process of resin used in correction fluid, by controlling various monomers, catalyst
With the usage ratio of the reagents such as solvent and the specific reaction condition of control, the painting with preferable caking property and dispersiveness is prepared for
Change resin used in liquid.Meanwhile to prevent from generating implode phenomenon since reaction speed is too fast in polymerization process, material goes out reaction
Container, present invention employs the methods that monomer is added portionwise, and ensure that reacting balance carries out.
Resin used in the correction fluid prepared according to the method for the embodiment of the present invention is added to as link stuff in correction fluid,
The correction fluid haveing excellent performance is made.During actual correction, gained alters the rapid levelling of liquid energy and insoluble writing, in dry coating
Row pen is smooth during upper writing, will not writing is not smooth when coating is too soft, occur dragging a phenomenon, coating will not rupture due to writing；
Gained correction fluid is placed 1 year even longer time, no lamination and is occurred simultaneously.
Description of the drawings
Fig. 1 is the flow chart of the chemical synthesis process of resin used in a kind of correction fluid described in the embodiment of the present invention.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, it is below in conjunction with the accompanying drawings and specific real
Applying mode, the present invention is described in further detail.
The realization flow of the method for the invention is described in detail below by embodiment.
Reference Fig. 1 shows the stream of the chemical synthesis process of resin used in a kind of correction fluid described in the embodiment of the present invention
Cheng Tu, as shown in Figure 1, the chemical synthesis process comprise the following steps：
Step 101, with two in methyl methacrylate, butyl acrylate, Isooctyl acrylate monomer and hydroxy-ethyl acrylate
Kind or more as soft monomer, for styrene as hard monomer, azodiisobutyronitrile is catalyst, and hexamethylene is solvent, is heated to reflux
The first mix monomer being made of the soft monomer, the hard monomer, the catalyst and the solvent, reaction generation first are mixed
Close liquid.
In first mix monomer, the methyl methacrylate and the mass ratio of the styrene stated is 0.117
~0.162, the mass ratio of the butyl acrylate and the styrene is 0.157~0.244, the hydroxy-ethyl acrylate and institute
The mass ratio of styrene is stated as 0.08~0.139, the mass ratio of the Isooctyl acrylate monomer and the styrene for 0.591~
0.75, the mass ratio of the azodiisobutyronitrile and the styrene is 0.014~0.031, the hexamethylene and the benzene second
The mass ratio of alkene is 1.909~2.778.
Conventional method uses benzoyl peroxide as catalyst, but benzoyl peroxide stability is poor, and by-product is more,
So present invention employs the azodiisobutyronitrile that stability is good, by-product is few as catalyst.
Common solvent has dichloroethanes, trichloroethanes, tetrachloroethanes, ethyl acetate and isopropanol etc., when using solvent
Larger harm can be generated to human body, the method for the embodiment of the present invention makees solvent using hexamethylene, and smell is also small, harm to the human body
It is small.
Step 102, second be made of the soft monomer and the hard monomer is slowly added dropwise into first mixed liquor
Mix monomer is added dropwise in 2~4h, obtains the second mixed liquor.
In second mix monomer, the mass ratio for stating methyl methacrylate and the styrene for 0.1~
0.148, the mass ratio of the butyl acrylate and the styrene is 0.143~0.222, the hydroxy-ethyl acrylate with it is described
The mass ratio of styrene is 0.074~0.11, the mass ratio of the Isooctyl acrylate monomer and the styrene for 0.524~
0.654。
Step 103, azodiisobutyronitrile is added in into second mixed liquor, flow back 3~4h, after reaction, cooling
To 30~40 DEG C of dischargings, resin used in the correction fluid is obtained.
The mass ratio of azodiisobutyronitrile wherein in step 103 and the styrene in step 102 is 0.01~0.022.
The present invention provides a kind of chemical synthesis process of resin used in correction fluid, by controlling various monomers, catalyst
With the usage ratio of the reagents such as solvent and the specific reaction condition of control, the painting with preferable caking property and dispersiveness is prepared for
Change resin used in liquid.Meanwhile to prevent from generating implode phenomenon since reaction speed is too fast in polymerization process, material goes out reaction
Container, present invention employs the methods that monomer is added portionwise, and ensure that reacting balance carries out.
In the embodiment of the present invention, it is preferable that first mix monomer and the monomer kind contained by second mix monomer
Class is identical.
The present invention also provides resins used in a kind of correction fluid, and resin passes through used in above-mentioned correction fluid used in the correction fluid
It is prepared by the chemical synthesis process of resin；
Resin used in the correction fluid has viscosity and dispersiveness.
Resin used in the correction fluid of synthesis has preferable filming performance, plays adherency as the bonding agent in correction fluid
With the effect of scattered covering agent.
The present invention also provides a kind of correction fluid, the resin included in the correction fluid is by tree used in above-mentioned correction fluid
Resin used in correction fluid prepared by the chemical synthesis process of fat；
After coating is dry, coating will not rupture the correction fluid because of writing, be not in drag a phenomenon；
The correction fluid is placed for a long time to be occurred without lamination.
Resin obtained is thick liquid mixture according to the method for the embodiment of the present invention, using the resin of preparation as connection
Material is added in correction fluid, is added the reagents such as titanium dioxide, auxiliary material and is ground, the correction fluid being had excellent performance.
During actual correction, gained alters the rapid levelling of liquid energy and insoluble writing, the row pen when being write on dry coating
Smoothness, will not writing is not smooth when coating is too soft, occur dragging a phenomenon, coating will not rupture due to writing；Gained is altered simultaneously
Liquid is placed 1 year even longer time, no lamination and is occurred.
For those skilled in the art is made to more fully understand the present invention, illustrate this hair below by way of multiple specific embodiments
The chemical synthesis process of resin used in the correction fluid of bright embodiment.
Embodiment 1
21 kilograms of methyl methacrylate, 44 kilograms of butyl acrylate, Isooctyl acrylate monomer are added in 2000L reaction kettles
109 kilograms, 180 kilograms of styrene, 500 kilograms of hexamethylene, 3.8 kilograms of azodiisobutyronitrile is heated to 90 DEG C or so and returned
Stream operation, reacts 2h.
18 kilograms of the monomers methyl methacrylate mixed is slowly added dropwise, 40 kilograms of butyl acrylate, acrylic acid is different pungent
101 kilograms of ester, 180 kilograms of styrene, drips off in 2h.
3 kilograms of azodiisobutyronitrile is added in, 90 DEG C or so progress reflux operations is heated to, reacts 4h, treat after reaction,
It is cooled to 35~40 DEG C of dischargings, obtains resin used in correction fluid.
Embodiment 2
22 kilograms of hydroxy-ethyl acrylate, 150 kilograms of Isooctyl acrylate monomer, 200 public affairs of styrene are added in 2000L reaction kettles
Jin, 500 kilograms of hexamethylene, 4.5 kilograms of azodiisobutyronitrile are heated to 95 DEG C or so progress reflux operations, react 1h.
20 kilograms of the monomeric acrylic hydroxyl ethyl ester mixed, 142 kilograms of Isooctyl acrylate monomer, styrene 217 is slowly added dropwise
Kilogram mix monomer is dripped off in 4h.
4 kilograms of azodiisobutyronitrile is added in, 95 DEG C or so progress reflux operations is heated to, reacts 3h, treat after reaction,
It is cooled to 30~35 DEG C of dischargings, obtains resin used in correction fluid.
Embodiment 3
34 kilograms of methyl methacrylate, 33 kilograms of butyl acrylate, Isooctyl acrylate monomer are added in 2000L reaction kettles
131 kilograms, 210 kilograms of styrene, 443 kilograms of hexamethylene, 6.3 kilograms of azodiisobutyronitrile is heated to 90~95 DEG C and returned
Stream operation, reacts 1.5h.
31 kilograms of the monomers methyl methacrylate mixed is slowly added dropwise, 30 kilograms of butyl acrylate, acrylic acid is different pungent
110 kilograms of ester, 210 kilograms of styrene, drips off in 3h.
3.5 kilograms of azodiisobutyronitrile is added in, 90~95 DEG C of progress reflux operations is heated to, 4h is reacted, to the end of reaction
Afterwards, it is cooled to 30~40 DEG C of dischargings, obtains resin used in correction fluid.
Embodiment 4
28 kilograms of methyl methacrylate, 40 kilograms of butyl acrylate, Isooctyl acrylate monomer are added in 2000L reaction kettles
120 kg, 203 kilograms of styrene, 475 kilograms of hexamethylene, 4.7 kilograms of azodiisobutyronitrile are heated to flowing back, and react 2h.
27 kilograms of the monomers methyl methacrylate mixed is slowly added dropwise, 39 kilograms of butyl acrylate, acrylic acid is different pungent
117 kilograms of ester, 200 kilograms of styrene, drips off in 2h.
4 kilograms of azodiisobutyronitrile is added in, flow back 3.5h, treats after reaction, to be cooled to 35~40 DEG C of dischargings, altered
Resin used in liquid.
Embodiment 5
18 kilograms of hydroxy-ethyl acrylate, 160 kilograms of Isooctyl acrylate monomer, 220 public affairs of styrene are added in 2000L reaction kettles
Jin, 420 kilograms of hexamethylene, 3 kilograms of azodiisobutyronitrile are heated to flowing back, and react 1.5h.
17 kilograms of the monomeric acrylic hydroxyl ethyl ester mixed, 138 kilograms of Isooctyl acrylate monomer, styrene 230 is slowly added dropwise
Kilogram mix monomer is dripped off in 3h.
5 kilograms of azodiisobutyronitrile is added in, flow back 3h, treats after reaction, to be cooled to 30~40 DEG C of dischargings, obtain correction fluid
Resin used.
Embodiment 6
25 kilograms of hydroxy-ethyl acrylate, 130 kilograms of Isooctyl acrylate monomer, 180 public affairs of styrene are added in 2000L reaction kettles
Jin, 460 kilograms of hexamethylene, 5.5 kilograms of azodiisobutyronitrile are heated to flowing back, and react 2h.
22 kilograms of the monomeric acrylic hydroxyl ethyl ester mixed, 130 kilograms of Isooctyl acrylate monomer, styrene 200 is slowly added dropwise
Kilogram mix monomer is dripped off in 2h.
2 kilograms of azodiisobutyronitrile is added in, flow back 4h, treats after reaction, to be cooled to 30~35 DEG C of dischargings, obtain correction fluid
Resin used.
Above to tree used in the chemical synthesis process of resin used in a kind of correction fluid provided by the present invention, a kind of correction fluid
Fat and a kind of correction fluid are described in detail, specific case used herein to the principle of the present invention and embodiment into
Elaboration is gone, the explanation of above example is only intended to help to understand the method and its core concept of the present invention；Meanwhile for this
The those skilled in the art in field, thought according to the invention, there will be changes in specific embodiments and applications,
In conclusion this specification content should not be construed as limiting the invention.
Claims (4)
1. the chemical synthesis process of resin used in a kind of correction fluid, which is characterized in that comprise the following steps：
Step (1), it is different pungent at least one of methyl methacrylate, butyl acrylate and hydroxy-ethyl acrylate and acrylic acid
The combination of ester is as soft monomer, and for styrene as hard monomer, azodiisobutyronitrile is catalyst, and hexamethylene is solvent, is heated back
The first mix monomer being made of the soft monomer, the hard monomer, the catalyst and the solvent is flowed, reacts 1~2h, it is raw
Into the first mixed liquor,
In first mix monomer, the mass ratio of the methyl methacrylate and the styrene for 0.117~
0.162, the mass ratio of the butyl acrylate and the styrene is 0.157~0.244, the hydroxy-ethyl acrylate with it is described
The mass ratio of styrene is 0.08~0.139, the mass ratio of the Isooctyl acrylate monomer and the styrene for 0.591~
0.75, the mass ratio of the azodiisobutyronitrile and the styrene is 0.014~0.031, the hexamethylene and the benzene second
The mass ratio of alkene is 1.909~2.778；
The second mixing being made of the soft monomer and the hard monomer is slowly added dropwise into first mixed liquor for step (2)
Monomer is added dropwise in 2~4h, obtains the second mixed liquor,
In second mix monomer, the mass ratio of the methyl methacrylate and the styrene is 0.1~0.148,
The mass ratio of the butyl acrylate and the styrene is 0.143~0.222, the hydroxy-ethyl acrylate and the styrene
Mass ratio for 0.074~0.11, the mass ratio of the Isooctyl acrylate monomer and the styrene is 0.524~0.654；
Step (3) adds in azodiisobutyronitrile into second mixed liquor, and flow back 3~4h, after reaction, is cooled to 30
~40 DEG C of dischargings, obtain resin used in the correction fluid, wherein the azodiisobutyronitrile in the step (3) and the step
Suddenly the mass ratio of the styrene in (2) is 0.01~0.022.
2. chemical synthesis process according to claim 1, which is characterized in that first mix monomer is mixed with described second
The monomeric species closed contained by monomer are identical.
3. resin used in a kind of correction fluid, which is characterized in that resin used in the correction fluid passes through any one of claim 1~2
It is prepared by the method；
Resin used in the correction fluid has viscosity and dispersiveness.
4. a kind of correction fluid, which is characterized in that the resin included in the correction fluid is passes through any one of claim 1~2 institute
State resin used in the correction fluid of method preparation；
After coating is dry, coating will not rupture the correction fluid because of writing, be not in drag a phenomenon；
The correction fluid is placed for a long time to be occurred without lamination.
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| CN201610071257.5A CN105566548B (en) | 2016-02-01 | 2016-02-01 | Resin and its chemical synthesis process used in a kind of correction fluid and a kind of correction fluid |
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| CN101045837A (en) * | 2007-04-27 | 2007-10-03 | 上海乐美文具有限公司 | Water-base correction fluid composite and preparation method thereof |
| CN102964530A (en) * | 2012-12-28 | 2013-03-13 | 陕西科技大学 | Aqueous correction fluid free of organic solvent and preparation method thereof |
| CN103224579A (en) * | 2013-04-03 | 2013-07-31 | 华东理工大学 | Method of preparing low-molecular-weight styrene-acrylate emulsion copolymer |
| CN103554344A (en) * | 2013-09-30 | 2014-02-05 | 上海乘鹰新材料有限公司 | Synthetic method of transparent water-whitening resistant polyacrylate emulsion |
| CN103992428A (en) * | 2013-02-19 | 2014-08-20 | 上海飞凯光电材料股份有限公司 | Acrylate resin, preparation method and application thereof |
| CN104311727A (en) * | 2014-11-06 | 2015-01-28 | 任婧 | Acrylic resin for transfer ink |
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2016
- 2016-02-01 CN CN201610071257.5A patent/CN105566548B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101045837A (en) * | 2007-04-27 | 2007-10-03 | 上海乐美文具有限公司 | Water-base correction fluid composite and preparation method thereof |
| CN102964530A (en) * | 2012-12-28 | 2013-03-13 | 陕西科技大学 | Aqueous correction fluid free of organic solvent and preparation method thereof |
| CN103992428A (en) * | 2013-02-19 | 2014-08-20 | 上海飞凯光电材料股份有限公司 | Acrylate resin, preparation method and application thereof |
| CN103224579A (en) * | 2013-04-03 | 2013-07-31 | 华东理工大学 | Method of preparing low-molecular-weight styrene-acrylate emulsion copolymer |
| CN103554344A (en) * | 2013-09-30 | 2014-02-05 | 上海乘鹰新材料有限公司 | Synthetic method of transparent water-whitening resistant polyacrylate emulsion |
| CN104311727A (en) * | 2014-11-06 | 2015-01-28 | 任婧 | Acrylic resin for transfer ink |
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