CN103436178A - Long-term storage method of rosin pentaerythritol ester - Google Patents
Long-term storage method of rosin pentaerythritol ester Download PDFInfo
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- CN103436178A CN103436178A CN2013103970293A CN201310397029A CN103436178A CN 103436178 A CN103436178 A CN 103436178A CN 2013103970293 A CN2013103970293 A CN 2013103970293A CN 201310397029 A CN201310397029 A CN 201310397029A CN 103436178 A CN103436178 A CN 103436178A
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- pentalyn
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- prolonged storage
- pentaerythritol ester
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Abstract
The invention discloses a long-term storage method of rosin pentaerythritol ester. The long-term storage method comprises the following steps of: rosin pentaerythritol ester discharging, moulding, packaging and the like; the contact of the rosin pentaerythritol ester with oxygen in air is blocked, oxygen dissolved in the rosin pentaerythritol ester is reduced and avoided, and an oxidizing reaction which is possible to take place during long-term storage is avoided; meanwhile an antioxidant is added and thoroughly dispersed on the surface of the product to form a protective layer; therefore, the stability and weather fastness of the rosin pentaerythritol ester are improved, and the color of colorless or pale rosin pentaerythritol ester product can be remained for a long time without changing.
Description
Technical field
The invention belongs to the pentalyn technical field, relate in particular to a kind of pentalyn prolonged storage method.
Background technology
Pentalyn is a kind of rosin deep processed product obtained by rosin and tetramethylolmethane reaction, and it is widely used in the fields such as coating, printing ink, sizing agent, emulsion.
The color of pentalyn plays very crucial effect to its product price and the market competitiveness, and colourless and pale rosin modified product is one of important both at home and abroad development research content.Preparation method and the existing large quantity research of technology about colourless and pale rosin pentaerythritol ester.In order to make pentalyn that stability, weathering resistance preferably be arranged, by adding thermo-stabilizer and photostabilizer, the oxidisability of product is improved, be significantly improved as Chinese patent " high stability color-less rosin pentaerythrite ester and preparation method thereof " (200510095092.7 open days on Mays 17th, 2006 of the patent No.) has added stability and the weathering resistance of product after oxidation inhibitor and stablizer.Although the color-less rosin pentaerythrite ester that existing method obtains has stability preferably, still colour-change can occur in prolonged storage and long-distance transport, can not meet the requirement of international trade.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of technique is simple, easy handling, pentalyn prolonged storage method that production cost is low, to guarantee the pentalyn product, keeps the color of better quality in the prolonged storage process.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
Pentalyn prolonged storage method comprises the following steps:
<1 > rosin has reacted the pentalyn that makes when high temperature discharging with tetramethylolmethane, and the blocking-up product contacts with atmospheric oxygen;
<2 > under protection of inert gas, by step<1 > pentalyn that obtains is prepared into sheet, granular or powder-like product;
<3 > by step<2 > the pentalyn product that makes mixes with oxidation inhibitor, makes oxidation inhibitor be well dispersed in product surface and form protective layer;
<4 > through step<3 > the pentalyn product processed is when packing, and the blocking-up product contacts with atmospheric oxygen.
Step<1 > or<4 in the blocking-up product with atmospheric oxygen, contact adopt vacuum, decompression, protection of inert gas or reduce pressure under the mode of protection of inert gas.
Rare gas element comprises nitrogen, carbonic acid gas, helium.
The oxidation inhibitor consumption is 0～1.0% of pentalyn quality.
Oxidation inhibitor is 2,2'-methylene-bis (4-methyl-6-tert-butylphenol), four [methylene radical β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 4,4'-butyl two (3 methy 6 tert butyl phenol), 1, one or more in 1,3-tri-(2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane, phosphorous acid dihydroxyphenyl propane ester.
Step<4 > the middle packing bag that adopts the sealing lucifuge.
Be long placed in the problem of variable color for current colourless and pale rosin pentaerythritol ester, the contriver has set up a kind of pentalyn prolonged storage method, in pentalyn discharging, moulding, packaging and other steps, by the blocking-up pentalyn, with atmospheric oxygen, contact, reduce and avoided oxygen dissolution in pentalyn, oxidizing reaction occurs while having avoided prolonged storage; Add oxidation inhibitor simultaneously and make it be well dispersed in product surface formation protective layer, thereby improved stability and the weathering resistance of pentalyn, color colourless or pale rosin pentaerythritol ester product can be kept and nondiscoloration for a long time.
Embodiment
Embodiment 1
<1 > rosin has reacted the pentalyn (color is less than for No. Ha Sense No. 150) that makes when high temperature discharging with tetramethylolmethane, adopts vacuum mode blocking-up product to contact with atmospheric oxygen;
<2 > under nitrogen protection, by step<1 > pentalyn that obtains is prepared into granulated product;
<3 > by step<2 > the pentalyn product that makes and 2,2'-methylene-bis (4-methyl-6-tert-butylphenol) (0.5%) mix, make oxidation inhibitor be well dispersed in product surface and form protective layer;
<4 > through step<3 > the pentalyn product of processing adopts the package bag vacuum packing of sealing lucifuge, during packing, adopts vacuum mode blocking-up product to contact with atmospheric oxygen.
Under room temperature, place 6 months, color is less than for No. Ha Sense No. 300, and room temperature is placed 12 months color Ghana looks number and is less than No. 1.
Embodiment 2
<1 > rosin has reacted the pentalyn (color is less than for No. Ha Sense No. 150) that makes when high temperature discharging with tetramethylolmethane, adopts vacuum mode blocking-up product to contact with atmospheric oxygen;
<2 > under nitrogen protection, by step<1 > pentalyn that obtains is prepared into granulated product;
<3 > through step<2 > the pentalyn product of processing adopts the package bag vacuum packing of sealing lucifuge, during packing, adopts vacuum mode blocking-up product to contact with atmospheric oxygen.
Under room temperature, place 6 months, Ghana's look number is less than No. 1, and room temperature is placed 12 months color Ghana looks number and is less than No. 2.
Embodiment 3
<1 > rosin has reacted the pentalyn (color is less than for No. Ha Sense No. 150) that makes when high temperature discharging with tetramethylolmethane, adopts vacuum mode blocking-up product to contact with atmospheric oxygen;
<2 > under nitrogen protection, by step<1 > pentalyn that obtains is prepared into flaked product;
<3 > by step<2 > pentalyn product and 0.05% 4 [methylene radical β-(3 that make, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and 0.05%4,4'-butyl two (3 methy 6 tert butyl phenol) mixes, and makes oxidation inhibitor be well dispersed in product surface and forms protective layer;
<4 > through step<3 > the pentalyn product of processing adopts the package bag vacuum packing of sealing lucifuge, during packing, adopts vacuum mode blocking-up product to contact with atmospheric oxygen.
Under room temperature, place 6 months, color is less than for No. Ha Sense No. 300, and room temperature is placed 12 months color Ghana looks number and is less than No. 1.
Embodiment 4
<1 > rosin has reacted the pentalyn (color is less than for No. Ha Sense No. 150) that makes when high temperature discharging with tetramethylolmethane, adopts vacuum mode blocking-up product to contact with atmospheric oxygen;
<2 > under nitrogen protection, by step<1 > pentalyn that obtains is prepared into granulated product;
<3 > by step<2 > the pentalyn product that makes mixes with 0.1%1,1,3-tri-(2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane and 0.2% phosphorous acid dihydroxyphenyl propane ester, makes oxidation inhibitor be well dispersed in product surface and form protective layer;
<4 > through step<3 > the pentalyn product of processing adopts the package bag vacuum packing of sealing lucifuge, during packing, adopts vacuum mode blocking-up product to contact with atmospheric oxygen.
Under room temperature, place 6 months, color is less than for No. Ha Sense No. 300, and room temperature is placed 12 months color Ghana looks number and is less than No. 1.
Embodiment 5
<1 > rosin has reacted the pentalyn (color is less than for No. Ha Sense No. 150) that makes when high temperature discharging with tetramethylolmethane, adopts vacuum mode blocking-up product to contact with atmospheric oxygen;
<2 > under carbon-dioxide protecting, by step<1 > pentalyn that obtains is prepared into granulated product;
<3 > by step<2 > the pentalyn product that makes mixes with 0.1%1,1,3-tri-(2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane and 0.2% phosphorous acid dihydroxyphenyl propane ester, makes oxidation inhibitor be well dispersed in product surface and form protective layer;
<4 > through step<3 > the pentalyn product of processing adopts the packaging bags of sealing lucifuge, during packing, pours carbonic acid gas blocking-up product and contacts with atmospheric oxygen, packs mouth;
Under room temperature, place 6 months, color is less than for No. Ha Sense No. 300, and room temperature is placed 12 months color Ghana looks number and is less than No. 1.
Embodiment 6
<1 > rosin has reacted the pentalyn (color is less than for No. Ha Sense No. 150) that makes when high temperature discharging with tetramethylolmethane, adopts vacuum mode blocking-up product to contact with atmospheric oxygen;
<2 > under nitrogen protection, by step<1 > pentalyn that obtains is prepared into granulated product;
<3 > by step<2 > the pentalyn product that makes and 1,1,3-tri-(2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane (1.0%) mix, make oxidation inhibitor be well dispersed in product surface and form protective layer;
<4 > through step<3 > the pentalyn product of processing adopts the packaging bags of sealing lucifuge, during packing, pours nitrogen blocking-up product and contacts with atmospheric oxygen, packs mouth;
Under room temperature, place 6 months, color is less than for No. Ha Sense No. 150, and room temperature is placed 12 months color Ghana looks number and is less than No. 1.
Comparative Examples 1
Rosin is to be less than pentalyn for No. Ha Sense No. 150 with making color after tetramethylolmethane has reacted, and it is prepared to granulated product.
Under room temperature, place 1 month, color Ghana look number is greater than No. 1, under room temperature, places 3 months, and color Ghana look number is greater than No. 3, and room temperature is placed 12 months color Ghana looks number and is greater than No. 5.
Comparative Examples 2
Rosin is with after tetramethylolmethane has reacted, add 0.5% thermo-stabilizer 2, the 5-ditert-butylhydro quinone, it is to be less than the pentalyn of No. 150 No. Ha Sense that 0.5% photostabilizer Octabenzone makes color, and it is made to granulated product.
Under room temperature, place 3 months, color is received look number for No. Ha Sense and is greater than No. 1, and room temperature is placed 12 months color Ghana looks number and is greater than No. 5.
Make high stability color-less rosin pentaerythrite ester by Chinese patent " high stability color-less rosin pentaerythrite ester and preparation method thereof " (200510095092.7 open days on Mays 17th, 2006 of the patent No.); with Double-layer packaging bag, pack; under room temperature sealing lucifuge, without the traditional method of adding oxidation inhibitor, vacuum, decompression, protection of inert gas processing, stored.Carry out the long-term storage comparative experiments with the pentalyn of processing through the present invention, result is as shown in table 1.
Table 1 product long-term storage effect
Visible, even high stability color-less rosin pentaerythrite ester, if not carrying out oxygen blocking processing and oxidation inhibitor processes and stores by traditional method, product just starts to see obvious colour-change in 3 months, after 6 months, sheet and granulated product color are darker, be (Ghana's look number) more than 3, powder-product reaches (Ghana's look number) more than 4.And employing the present invention, it is very little that product stores colour-change for a long time, even after December, color still is less than 1(Ghana look number).
Claims (6)
1. a pentalyn prolonged storage method is characterized in that comprising the following steps:
<1 > rosin has reacted the pentalyn that makes when high temperature discharging with tetramethylolmethane, and the blocking-up product contacts with atmospheric oxygen;
<2 > under protection of inert gas, by step<1 > pentalyn that obtains is prepared into sheet, granular or powder-like product;
<3 > by step<2 > the pentalyn product that makes mixes with oxidation inhibitor, makes oxidation inhibitor be well dispersed in product surface and form protective layer;
<4 > through step<3 > the pentalyn product processed is when packing, and the blocking-up product contacts with atmospheric oxygen.
2. pentalyn prolonged storage method according to claim 1, is characterized in that step<1 > or<4 in the blocking-up product with atmospheric oxygen, contact adopt vacuum, decompression, protection of inert gas or reduce pressure under the mode of protection of inert gas.
3. pentalyn prolonged storage method according to claim 2, it is characterized in that: described rare gas element comprises nitrogen, carbonic acid gas, helium.
4. pentalyn prolonged storage method according to claim 3, it is characterized in that: described oxidation inhibitor consumption is 0～1.0% of pentalyn quality.
5. pentalyn prolonged storage method according to claim 4, it is characterized in that: described oxidation inhibitor is 2,2'-methylene-bis (4-methyl-6-tert-butylphenol), four [methylene radical β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 4,4'-butyl two (3 methy 6 tert butyl phenol), 1, one or more in 1,3-tri-(2-methyl-4-hydroxyl-5-tert-butyl-phenyl) butane, phosphorous acid dihydroxyphenyl propane ester.
6. pentalyn prolonged storage method according to claim 5, is characterized in that step<4 > the middle packing bag that adopts the sealing lucifuge.
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| CN2013103970293A CN103436178A (en) | 2013-09-04 | 2013-09-04 | Long-term storage method of rosin pentaerythritol ester |
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| CN2013103970293A CN103436178A (en) | 2013-09-04 | 2013-09-04 | Long-term storage method of rosin pentaerythritol ester |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527262A (en) * | 2019-09-16 | 2019-12-03 | 苏州宝丽迪材料科技股份有限公司 | Photochromic polyester fiber master batch and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110213120A1 (en) * | 2010-03-01 | 2011-09-01 | Arizona Chemical Company | Rosin esters for non-woven applications, methods of making and using and products therefrom |
| CN102964577A (en) * | 2012-11-30 | 2013-03-13 | 浙江鑫松树脂有限公司 | High-temperature-resistant rosin modified resin and production method thereof |
| CN103214971A (en) * | 2013-04-28 | 2013-07-24 | 上思县松香厂 | Preparation method of pale rosin ester |
-
2013
- 2013-09-04 CN CN2013103970293A patent/CN103436178A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110213120A1 (en) * | 2010-03-01 | 2011-09-01 | Arizona Chemical Company | Rosin esters for non-woven applications, methods of making and using and products therefrom |
| US20130197187A1 (en) * | 2010-03-01 | 2013-08-01 | Arizona Chemical Company, Llc | Rosin Esters for Non-Woven Applications, Methods of Making and Using and Products Therefrom |
| CN102964577A (en) * | 2012-11-30 | 2013-03-13 | 浙江鑫松树脂有限公司 | High-temperature-resistant rosin modified resin and production method thereof |
| CN103214971A (en) * | 2013-04-28 | 2013-07-24 | 上思县松香厂 | Preparation method of pale rosin ester |
Non-Patent Citations (2)
| Title |
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| 刘自力: "《林产化工产品生产技术》", 31 May 2005, 江西科学技术出版社 * |
| 高宏: "《松香酯的无色化和稳定化研究》", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527262A (en) * | 2019-09-16 | 2019-12-03 | 苏州宝丽迪材料科技股份有限公司 | Photochromic polyester fiber master batch and preparation method thereof |
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Application publication date: 20131211 |