CN103554804B - The preparation method of high intensity level acrylic tapetum lucidum supporting layer resin - Google Patents
The preparation method of high intensity level acrylic tapetum lucidum supporting layer resin Download PDFInfo
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- CN103554804B CN103554804B CN201310469036.XA CN201310469036A CN103554804B CN 103554804 B CN103554804 B CN 103554804B CN 201310469036 A CN201310469036 A CN 201310469036A CN 103554804 B CN103554804 B CN 103554804B
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Abstract
The invention discloses a kind of preparation method of high intensity level acrylic tapetum lucidum supporting layer resin, comprise the steps: (1), synthesis hard acrylic resin; (2), soft propylene acid resin is synthesized; (3), component is blended.The present invention fills a prescription rationally, and the cellulose acetate butyrate resin of use can improve the levelling property supporting resin, suppresses sagging and shrinkage cavity thus reduces surface imperfection, shortening time of drying.High intensity level acrylic tapetum lucidum prepared by the present invention has fabulous rebound resilience, tensile strength, oil-proofness, high high-low temperature resistant bandha, water-fast, acid and alkali-resistance, salt fog resistance.
Description
Technical field
The invention belongs to resin technology field, relate to a kind of preparation method of tapetum lucidum resin, be specifically related to a kind of preparation method of high intensity level acrylic tapetum lucidum supporting layer resin.
Background technology
20 beginnings of the century, U.S. doctor Dong Qifang of Chinese origin invents and have developed tapetum lucidum technology, is applied to road signs production.Its night is remote visibility under light-illuminating, by the widespread use of traffic safety industry.
Tapetum lucidum utilizes optical principle, light reflex reflection can be got back to the blooming of a kind of special construction at light source place.Be made up of the good thin film layer of weather resistance, tiny glass beads layer, reflecting layer, adhesive-layer and peel ply.
According to the road traffic tapetum lucidum GB/T18833-2012 standard of the up-to-date formulation of China, high-strength reflecting film is classified as three grades of films, it is a kind of high durable capsule-type tapetum lucidum, glistening intensity exceeds three times than engineering grade tapetum lucidum, high-strength reflecting film is for making different kinds of roads traffic mark board, be applicable to motorway, one-level, secondary, three grades, the road and traffic sign plates such as level Four, be generally 10 years work-ing life, this tapetum lucidum uses under normal circumstances, and after 10 years, its glistening intensity retention value is at least 80% of its initial stage glistening intensity.
Present domestic production height intensity level acrylic tapetum lucidum supporting layer is all use the processing of PU hot melt adhesive, and shortcoming is that PU hot melt adhesive long-term weatherability performance is bad, the poor and low temperature flexibility of acid and alkali-resistance solvent resistance and fume resistance poor.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of preparation method of high intensity level acrylic tapetum lucidum supporting layer resin, tapetum lucidum supporting layer resin prepared by the method has good performance.
Technical scheme of the present invention is as follows:
The preparation method of high intensity level acrylic tapetum lucidum supporting layer resin, the component of described acrylic tapetum lucidum supporting layer resin comprises hard acrylic resin, soft propylene acid resin, cellulose acetate butyrate resin and titanium dioxide, comprises the steps:
(1), hard acrylic resin is synthesized
The component of described hard acrylic resin comprises acrylic resin systems monomer, initiator and medium-boiling solvent;
During preparation, in reactor, first add the mix monomer of acrylic resin systems total monomer weight 40%, then add initiator and medium-boiling solvent, heat up 90 DEG C of solvent refluxings, the mix monomer of acrylic resin systems total monomer weight 60% is dripped at 95 DEG C, reaction times is 11 ~ 12 hours, when reaction conversion ratio is greater than 97%, continues isothermal reaction, when reaction conversion ratio reaches 99%, add solvent cut cooling fluid, be cooled within 30 DEG C, filter the discharging of hard acrylic resin;
(2), soft propylene acid resin is synthesized
The component of described soft propylene acid resin comprises acrylic resin systems monomer, initiator and high boiling solvent;
During preparation, in reactor, first add the mix monomer of acrylic resin systems total monomer weight 30%, then add initiator and high boiling solvent, heat up 150 DEG C of solvent refluxings, the mix monomer of acrylic resin systems monomer 70% is dripped at 150 DEG C, reaction times is 13 ~ 14 hours, when reaction conversion ratio is greater than 98%, continues isothermal reaction, when reaction conversion ratio reaches 99%, add solvent cut cooling fluid, be cooled within 30 DEG C, filter the discharging of soft propylene acid resin;
(3), component is blended
Get hard acrylic resin that above-mentioned steps (1) synthesizes and the soft propylene acid resin that step (2) is synthesized and cellulose acetate butyrate resin and titanium dioxide, can be formulated after even through high-speed stirring, static 24 hours.
On the basis of such scheme, in described acrylic tapetum lucidum supporting layer resin, the mass percent of each component is:
Hard acrylic resin: soft propylene acid resin: cellulose acetate butyrate resin: titanium dioxide=35:35:5:25.
As improvement of the present invention, described in step (1), hard acrylic resin comprises the component of following mass percent:
β-dimethyl-aminoethylmethacrylate monomer 30 ~ 40%, specific functional groups Acrylic Acid Monomer 10 ~ 15%, Acrylic Acid Monomer 7 ~ 10%, initiator 0.5 ~ 3%, medium-boiling solvent 40 ~ 60%.
Described in step (2), soft propylene acid resin comprises the component of following mass percent:
Acrylic acid ethyl ester monomer 35 ~ 40%, methyl methacrylate monomer 15 ~ 20%, special functional acrylic monomer 5 ~ 10%, initiator 0.5 ~ 2%, high boiling solvent 40 ~ 60%.
Further improve as the present invention, in above-mentioned steps (1), the molecular weight control of hard acrylic resin is in Mw (weight-average molecular weight)=55 ~ 1,000,000, and molecular weight distribution ratio Mw/Mn=15 ~ 20, molecular weight distribution is general.
In above-mentioned steps (2), soft acrylic molecular resin amount controls in Mw=50 ~ 600,000, and molecular weight distribution ratio Mw/Mn=20 ~ 30, molecular weight distribution is wider.
Bian gets technique scheme, and the beneficial effect that the present invention has is:
1, the present invention fills a prescription rationally, owing to employing cellulose acetate butyrate resin in formula, thus can improve the levelling property supporting resin, suppress sagging and shrinkage cavity thus reduce surface imperfection, shortening time of drying, promoting aligning of metallic pigment, solvent resistant corrodes, plasticizing agent migration resisting.
2, use PU with present tapetum lucidum supporting layer and have that hot melt adhesive long-term weatherability performance is poor, acid and alkali-resistance solvent resistance is poor and low temperature flexibility is poor, the shortcomings such as resistance to smog difference feature are different, high intensity level acrylic tapetum lucidum prepared by the present invention has fabulous rebound resilience, tensile strength, oil-proofness, high high-low temperature resistant bandha, water-fast, acid and alkali-resistance, salt fog resistance, reaches the requirement of GB/T18833-2012.
Embodiment
The preparation method of high intensity level acrylic tapetum lucidum supporting layer resin, comprises the steps:
(1), hard acrylic resin is synthesized
The component of described hard acrylic resin comprises acrylic resin systems monomer, initiator and medium-boiling solvent;
During preparation, take the mixture 1100.0g that β-dimethyl-aminoethylmethacrylate monomer 505.0g, specific functional groups Acrylic Acid Monomer (alkoxide nonylphenol acrylate) 200.5g, Acrylic Acid Monomer 120.0g, initiator Diisopropyl azodicarboxylate 25.0g, solvent use ethyl acetate and toluene mass ratio are 2:1;
In the jacket reactor of Dropping feeder that condensation reflux unit and flow control are housed, first add the total monomer weight 40% i.e. mix monomer of 330.2g, heat up 90 DEG C of solvent refluxings, drips mix monomer and the 495.3g of total monomer weight 60% at 95 DEG C; Reaction times is 11 ~ 12 hours, when reaction conversion ratio is greater than 97%, and continue isothermal reaction, reaction conversion ratio reaches 99%, adds solvent cut cooling fluid, is cooled within 30 DEG C, filters the discharging of hard acrylic resin;
(2), soft propylene acid resin is synthesized
The component of described soft propylene acid resin comprises acrylic resin systems monomer, initiator and high boiling solvent;
During preparation, take acrylic acid ethyl ester monomer 410.0g, specific functional groups Acrylic Acid Monomer (t-butyl cyclohexyl ester) 50.5g, methyl methacrylate monomer 180.0g, initiator Diisopropyl azodicarboxylate 20.0g, solvent use Solvesso100 and xylene mass than the mixture 900.0g being 1:1;
In the jacket reactor of Dropping feeder that condensation reflux unit and flow control are housed, first add the total monomer weight 30% i.e. mix monomer of 192.2g, heat up 150 DEG C of solvent refluxings, drips the total monomer weight 70% i.e. mix monomer of 448.4g at 150 DEG C; Reaction times is 13 ~ 14 hours, when reaction conversion ratio is greater than 98%, and continue isothermal reaction, reaction conversion ratio reaches 99%, adds solvent cut cooling fluid, is cooled within 30 DEG C, filters the discharging of soft propylene acid resin;
(3), component is blended
Get hard acrylic resin that above-mentioned steps (1) synthesizes and the soft propylene acid resin that step (2) is synthesized and cellulose acetate butyrate resin and titanium dioxide, can be formulated after even through high-speed stirring, static 24 hours.
Applicant states, person of ordinary skill in the field is on the basis of above-described embodiment, by the concrete content point value of above-described embodiment component, combined with the technical scheme of summary of the invention part, thus the new numerical range produced, also be one of record scope of the present invention, the application, for making specification sheets simple and clear, no longer enumerates these numerical ranges.
Claims (3)
1. the preparation method of high intensity level acrylic tapetum lucidum supporting layer resin, the component of described acrylic tapetum lucidum supporting layer resin comprises hard acrylic resin, soft propylene acid resin, cellulose acetate butyrate resin and titanium dioxide, the mass percent of each component is: hard acrylic resin: soft propylene acid resin: cellulose acetate butyrate resin: titanium dioxide=35:35:5:25, it is characterized in that, comprise the steps:
(1), hard acrylic resin is synthesized
The component of described hard acrylic resin comprises acrylic resin systems monomer, initiator and medium-boiling solvent, described hard acrylic resin comprises the component of following mass percent: β-dimethyl-aminoethylmethacrylate monomer 30 ~ 40%, alkoxide nonylphenol acrylate 10 ~ 15%, Acrylic Acid Monomer 7 ~ 10%, initiator 0.5 ~ 3%, medium-boiling solvent 40 ~ 60%, and in described hard acrylic resin, the mass percent sum of each component is 100%;
During preparation, in reactor, first add the mix monomer of acrylic resin systems total monomer weight 40%, then add initiator and medium-boiling solvent, heat up 90 DEG C of solvent refluxings, the mix monomer of acrylic resin systems total monomer weight 60% is dripped at 95 DEG C, reaction times is 11 ~ 12 hours, when reaction conversion ratio is greater than 97%, continues isothermal reaction, when reaction conversion ratio reaches 99%, add solvent cut cooling fluid, be cooled within 30 DEG C, filter the discharging of hard acrylic resin;
(2), soft propylene acid resin is synthesized
The component of described soft propylene acid resin comprises acrylic resin systems monomer, initiator and high boiling solvent; Described soft propylene acid resin comprises the component of following mass percent: acrylic acid ethyl ester monomer 35 ~ 40%, methyl methacrylate monomer 15 ~ 20%, t-butyl cyclohexyl ester 5 ~ 10%, initiator 0.5 ~ 2%, high boiling solvent 40 ~ 60%, and in described soft propylene acid resin, the mass percent sum of each component is 100%;
During preparation, in reactor, first add the mix monomer of acrylic resin systems total monomer weight 30%, then add initiator and high boiling solvent, heat up 150 DEG C of solvent refluxings, the mix monomer of acrylic resin systems monomer 70% is dripped at 150 DEG C, reaction times is 13 ~ 14 hours, when reaction conversion ratio is greater than 98%, continues isothermal reaction, when reaction conversion ratio reaches 99%, add solvent cut cooling fluid, be cooled within 30 DEG C, filter the discharging of soft propylene acid resin;
(3), component is blended
Get hard acrylic resin that above-mentioned steps (1) synthesizes and the soft propylene acid resin that step (2) is synthesized and cellulose acetate butyrate resin and titanium dioxide, can be formulated after even through high-speed stirring, static 24 hours.
2. the preparation method of high intensity level acrylic tapetum lucidum supporting layer resin according to claim 1, it is characterized in that: in described step (1), the molecular weight control of hard acrylic resin is in Mw=55 ~ 1,000,000, molecular weight distribution ratio Mw/Mn=15 ~ 20.
3. the preparation method of high intensity level acrylic tapetum lucidum supporting layer resin according to claim 1, it is characterized in that: in described step (2), the molecular weight control of soft propylene acid resin is in Mw=50 ~ 600,000, molecular weight distribution ratio Mw/Mn=20 ~ 30.
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| CN111154386A (en) * | 2020-01-16 | 2020-05-15 | 上海立邦长润发涂料有限公司 | Brushing LED transparent primer, preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1108179A (en) * | 1995-01-21 | 1995-09-13 | 浙江大学 | Reflection products made of composite high molecular material |
| CN102529261A (en) * | 2011-12-15 | 2012-07-04 | 绵阳龙华薄膜有限公司 | Light reflection film |
| CN202592864U (en) * | 2012-04-28 | 2012-12-12 | 晋江联兴反光材料有限公司 | Sealed directional reflective film |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4487770B2 (en) * | 2004-12-28 | 2010-06-23 | 株式会社クラレ | Curable resin composition and antireflection material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1108179A (en) * | 1995-01-21 | 1995-09-13 | 浙江大学 | Reflection products made of composite high molecular material |
| CN102529261A (en) * | 2011-12-15 | 2012-07-04 | 绵阳龙华薄膜有限公司 | Light reflection film |
| CN202592864U (en) * | 2012-04-28 | 2012-12-12 | 晋江联兴反光材料有限公司 | Sealed directional reflective film |
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