CN1261400C - Ultraviolet absorbent UV-1200 synthesis - Google Patents
Ultraviolet absorbent UV-1200 synthesis Download PDFInfo
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- CN1261400C CN1261400C CN 02157739 CN02157739A CN1261400C CN 1261400 C CN1261400 C CN 1261400C CN 02157739 CN02157739 CN 02157739 CN 02157739 A CN02157739 A CN 02157739A CN 1261400 C CN1261400 C CN 1261400C
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- absorbing agent
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Abstract
The present invention relates to a preparing method of an ultraviolet absorbing agent UV-1200 (the chemical name: 2-hydroxy-4-n-hexadecanedimethyl diphenyl methanone), which is characterized in that UV-0 (the chemical name: 2, 4-dihydroxydiphenyl methanone), front dodecyl alkyl halide and inorganic base react in 120 to 150 DEG C for 1 to 8 hours under the condition without any organic solvent to prepare the ultraviolet absorbing agent UV-1200 in high yield. Compared with other methods reported at home and abroad, the method has the outstanding advantage that organic solvents are not used, so a reaction technique is environment friendly. The method has the advantages of green technique, simple operation, low cost and high yield, and is suitable for large-scale commercial production.
Description
The present invention relates to the preparation method of uv-absorbing agent UV-1200.The chemical name of UV-1200: 2-hydroxyl-4-positive 12-alkoxy benzophenone (2-HYDROXYL-4-N-DODEOXY-BENZOPHENONE), molecular formula is C
25H
34O
3, structural formula is:
Uv-absorbing agent UV-1200 is the regeneration product of UV-531, UV-9.These product are nontoxic, nonflammable, non-explosive, burn into excellent storage stability not, can absorb the 270-340nm ultraviolet ray, prevent that photoaging, be full of cracks and embrittlement from appearring in macromolecular material, prolongs the work-ing life of material greatly.Because its performance brilliance, thereby be widely used in polyethylene, polypropylene, acrylic abroad, various high-grade paints and automobile finish.
In the existing synthetic method of domestic and foreign literature report, all adopt organic solvent or phase-transfer catalyst in the reaction system.(print during chemical industry, 1997 11 the 1st phases of volume, p28-30) report adopts in phase-transfer catalyst and the reaction and selects organic solvent for use the auspicious grade of profound scholar, and yield is 90%; Report such as Fernando J.Ponder (US3526666) solvent method yield is 60%.Adopt organic solvent and phase-transfer catalyst in the reaction, not only Financial cost rises, and residue problem is often arranged.
The production technique greenization has become an important directions of chemosynthesis, and the present invention adopts solventless method to prepare UV-1200.Its remarkable advantage is to avoid using poisonous organic solvent or catalyzer in the reaction, has realized the greenization of reaction process.Yield is about 90%.In this method technology green, simple to operate, cost is low, and the yield height is fit to large-scale commercial production.
The concrete synthetic route of the present invention can be expressed as:
Wherein, the dodecyl haloalkane is meant dodecyl bromide or dodecyl chlorine; Mineral alkali is meant sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, or their mixture.
The feed ratio of UV-0, dodecyl haloalkane, mineral alkali is mol ratio 1: 1.0-1.2: 1.0-5.0.Temperature of reaction is 120-150 ℃, and the reaction times is 1-8 hour.Aftertreatment is to adopt washing, to remove inorganic impurity, and further refining pure product.
Following examples help to understand the present invention, but do not limit range of application of the present invention.
Specific embodiment one:
Raw material UV-0 (214g, 1.0mol), C
12H
25Br (261g, 1.05mol), NaOH (40g, 1.0mol), K
2CO
3(136g 1.0mol) reacted 1.5 hours in 120-150 ℃ in the 1000ml reaction flask.After reaction finishes, add the 500ml washing and remove inorganic impurity, washing is repeatedly to neutral again.Further underpressure distillation of organic phase or recrystallization get white pure product 344g, and be fusing point 51-52 ℃, in full accord through identifying with n-compound.Yield is 90%.
Claims (4)
1. the synthetic method of uv-absorbing agent UV-1200 is characterized in that: 2,4 dihydroxyl benzophenone, dodecyl haloalkane, mineral alkali adopt the solventless method reaction, make uv-absorbing agent UV-1200 through aftertreatment again.
2. the synthetic method of uv-absorbing agent UV-1200 as claimed in claim 1, wherein the feed ratio of 2,4 dihydroxyl benzophenone, dodecyl haloalkane, mineral alkali is mol ratio 1: 1.0-1.2: 1.0-5.0.
3. the synthetic method of uv-absorbing agent UV-1200 as claimed in claim 1, wherein temperature of reaction is 120-150 ℃, the reaction times is 1-8 hour.
4. the synthetic method of uv-absorbing agent UV-1200 as claimed in claim 1, wherein aftertreatment is to adopt washing, to remove inorganic impurity, further refining pure product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157739 CN1261400C (en) | 2002-12-24 | 2002-12-24 | Ultraviolet absorbent UV-1200 synthesis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157739 CN1261400C (en) | 2002-12-24 | 2002-12-24 | Ultraviolet absorbent UV-1200 synthesis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1510022A CN1510022A (en) | 2004-07-07 |
| CN1261400C true CN1261400C (en) | 2006-06-28 |
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ID=34236674
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02157739 Expired - Fee Related CN1261400C (en) | 2002-12-24 | 2002-12-24 | Ultraviolet absorbent UV-1200 synthesis |
Country Status (1)
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| CN (1) | CN1261400C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629034B (en) * | 2009-08-03 | 2012-07-04 | 重庆大学 | Ultraviolet absorbent and preparation method thereof |
| CN102584727B (en) * | 2011-11-28 | 2015-04-29 | 江南大学 | Method for synthesizing novel reactive ultraviolet absorbent and application thereof |
| CN103508870A (en) * | 2013-09-24 | 2014-01-15 | 江苏紫奇化工科技有限公司 | UV-531 clean synthetic method |
| CN104098454A (en) * | 2014-07-25 | 2014-10-15 | 襄阳市金达成精细化工有限责任公司 | Production method of ultraviolet light absorber |
| CN112142581A (en) * | 2019-06-27 | 2020-12-29 | 江苏紫奇化工科技有限公司 | Process for synthesizing UV-531 from chloro-n-octane |
-
2002
- 2002-12-24 CN CN 02157739 patent/CN1261400C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1510022A (en) | 2004-07-07 |
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Effective date of registration: 20090213 Address after: 19E, 1 building 3500, Kai Po Road, Shanghai, zip code: 200030 Co-patentee after: Gaowei Science and Technology Development Co., Ltd., Shanghai Patentee after: Shanghai high dimensional Chemical Co., Ltd. Address before: No. 1669, triumph Road, Shanghai, 3 floor, zip code: 200030 Patentee before: Shanghai Gaowei Chemistry Co., Ltd. |
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Addressee: Shanghai Gaowei Chemistry Co., Ltd. Document name: Notification to Pay the Fees |
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Granted publication date: 20060628 Termination date: 20141224 |
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