CN101585910B - Process for preparing alkyd by using waste polyester bottle - Google Patents
Process for preparing alkyd by using waste polyester bottle Download PDFInfo
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- CN101585910B CN101585910B CN2008100160804A CN200810016080A CN101585910B CN 101585910 B CN101585910 B CN 101585910B CN 2008100160804 A CN2008100160804 A CN 2008100160804A CN 200810016080 A CN200810016080 A CN 200810016080A CN 101585910 B CN101585910 B CN 101585910B
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- synolac
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- tetramethylolmethane
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Abstract
The invention relates to a process for preparing alkyd by using a waste polyester bottle, the finished alkyd product is finally prepared by using the following raw materials according to the proportion after the esterification reaction: 20-25 percent of oil, 5.5-8.2 percent of polylol, 13-15 percent of polyester bottle, 2.5-3 percent of dimethylbenzene, 1-2 percent of maleic anhydride, 0-7 percent of rosin and 45-50 percent of No. 200 solvent oil. The invention has low production cost, obviously improves the property of the prepared alkyd, utilizes the waste resource and has better economic and social profit.
Description
Affiliated technical field
The present invention relates to paint the resin manufacture technology in the manufacturing, especially utilize waste polyester bottle to replace phthalic anhydride to prepare the technology of Synolac.
Background technology
Synolac is a kind of coating synthetic resins, may be used solely to system lacquer, for example makes priming paint, finish paint, varnish etc., also can with system lacquer after the mixed with resin of other classifications, of many uses.At present, the method for preparing Synolac commonly used is under the condition that catalyzer exists, and utilizes raw materials such as soya-bean oil, polyvalent alcohol and phthalic anhydride, makes through esterification.In recent years, be subjected to the influence of rise in oil price, the impetus that the raw material of preparation Synolac goes up is stronger, makes production cost greatly increase.Therefore, how to utilize low cost raw material to replace known raw material production Synolac, become the important content that people improve alkyd resin production technology, but this work makes little progress so far.Number of patent application is to disclose a kind of alkyd resin production technology of utilizing crude terephthalic acid to substitute most of phthalic anhydride in 200710021495.6 the application for a patent for invention Publication Specification, production cost is slightly reduced, but the crude terephthalic acid on the market still costs an arm and a leg, more than 8000 yuan per ton have been reached at present, and the Synolac that makes in this way, its result of use is also undesirable.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, provide a kind of waste polyester bottle that utilizes to substitute the technology that phthalic anhydride is made the feedstock production Synolac, this preparation method's production cost is low, and the resin result of use that makes is good.
For achieving the above object, the feature of technical solution of the present invention is to use following proportion raw material by weight percentage, after esterification, finally make the Synolac finished product: oily 20-25%, polyvalent alcohol 5.5-8.2%, polyester bottles 13-15%, dimethylbenzene 2.5-3%, MALEIC ANHYDRIDE 1-2%, rosin 0-7%, 200# solvent oil 45-50%, wherein MALEIC ANHYDRIDE is used as catalyzer.
The said oil of the present invention is meant refining soya-bean oil, soya-bean oil or acidifying oil; Said polyvalent alcohol is tetramethylolmethane and/or glycerine, and when selecting tetramethylolmethane for use separately, its weight percent is 6-7.5%, and when the two was selected for use simultaneously, its weight percent was respectively: glycerine 1.0-1.6%, tetramethylolmethane 4.5-6.5%.Also can add the lithium hydroxide of 0.007-0.01% (weight) in the reactant as antioxidant.
The present invention adopts and is prepared as follows step: add reactant oil and rosin in reaction vessel, afterwards under the condition of continuous attemperation, add tetramethylolmethane successively, alcoholysis to clear back adds polyester bottle slice, degraded adds MALEIC ANHYDRIDE, backflow dimethylbenzene to transparent back, esterification is incubated when viscosity is 3.5-10s (Ge Shi pipe, 25 ℃), acid value≤10mgKOH/g lowers the temperature, resultant is added 200# solvent oil latting drown, promptly make the Synolac finished product behind the elimination waste residue.
Above said continuous attemperation be meant: add tetramethylolmethane when temperature rises to 220 ℃, be warming up to 240 ℃ then, after alcoholysis is extremely clear, add polyester bottle slice when continuing to be warming up to 250 ℃, maintain the temperature at 250-260 ℃ of degraded after transparent, add MALEIC ANHYDRIDE, backflow dimethylbenzene when being cooled to 210 ℃, esterification insulation when being warming up to 230-240 ℃ then.
In the above-mentioned preparation process, also comprise glycerine in the reactant, can add the antioxidant lithium hydroxide when reactant is warming up to 120 ℃.
The present invention is the effective constituent polyethylene terephthalate that utilizes polyester beverage bottle, mineral water bottle, make it grafting in the Synolac system by edman degradation Edman, replace the main raw material phthalic anhydride in the original production process, then by refluxing xylene method control esterification temperature, the effective constituent polyethylene terephthalate that makes polyester bottles is after degraded, generate incomplete ester with oil and polyprotonic acid in the system through alcoholysis, under the effect of catalyzer, hydroxyl in the system, carboxyl are redistributed and are formed new polycondensation structure, thereby make modified alkyd resin.
The consumption of each reactant of the present invention only is the test adequate value, the consumption of polyester bottles for example, if consumption is lower than 13%, then the reaction times prolongs, and the resin transparent that makes is poor, if consumption is higher than 15%, then the reaction times shortens, but therefore the color of resin that makes intensification selects for use the consumption of 13-15% comparatively appropriate, but depart from a small quantity, still belong to scope of the present invention.Equally, temperature control in the preparation process also belongs to the test adequate value, for example add the degradation temperature after the polyester bottles, if temperature is lower than 250 ℃, then resin is unclear, and when temperature is higher than 260 ℃, degradation time shortens, the transparency of resin, but the investment that may increase high temperature service, so chooses 250-260 ℃ and be advisable, but this temperature value is not an accurate must value of the present invention.
One of beneficial effect of the present invention is to have reduced production cost.The present invention adopts the lower useless polyester beverage bottle of price to replace the higher raw material phthalic anhydride of price, and resin of every production can be saved more than 100 yuan of production cost, thereby makes production cost reduce greatly.Another beneficial effect of the present invention is that the performance of the Synolac that makes has had and significantly improves.In the former Synolac because of containing hydroxyl and carboxyl functional group, thereby water tolerance, resistance to salt water are relatively poor, and the effective constituent polyethylene terephthalate of the polyester beverage bottle that the present invention uses itself is exactly a kind of not labile high polymeric compound, relatively stronger stability and corrosion-resistant, weather resistance, anti-strong solvent are arranged, it is grafted in the Synolac can be the together good barrier of paint film increase of resin, thus the quality of raising alkyd paint.It is the utilization ratio that has improved scrap feed material that the present invention also has a beneficial effect, has saved resource, also can reduce the pollution of white garbage, has the good social benefit.
Embodiment
Embodiment 1, present embodiment adopt following proportioning raw materials by weight percentage: refining soya-bean oil 21%, glycerine 1.5%, lithium hydroxide 0.010%, tetramethylolmethane 5%, polyester bottles 20%, MALEIC ANHYDRIDE 2%, dimethylbenzene 2.8%, 200# solvent oil 45%.
The preparation process of present embodiment is as follows: will make with extra care soya-bean oil, glycerine adds intensification in the reactor, add the antioxidant lithium hydroxide during to 120 ℃, add tetramethylolmethane when continuing to be warming up to 220 ℃, insulation after being warming up to 240 ℃, add polyester bottle slice when being warming up to 250 ℃ after alcoholysis is extremely clear, maintain the temperature at 250-260 ℃, add MALEIC ANHYDRIDE when being cooled to 210 ℃ after degraded is extremely clear, backflow dimethylbenzene, and then be warming up to 230-240 ℃ and carry out esterification insulation, when viscosity is 7-10s (Ge Shi pipe, 25 ℃), during acid value≤10mgKOH/g, lowering the temperature still, add 200# solvent oil latting drown, promptly get the Synolac finished product after the filtration.The Synolac that present embodiment makes is particularly suitable for being used for preparing enamel paint, the synthetic enamel glossiness height that it is made, and anti-efflorescence, gloss retention are good.
Embodiment 2, present embodiment adopt the following raw materials according proportioning by weight percentage: soya-bean oil 24%, glycerine 1.2%, lithium hydroxide 0.01%, rosin 4%, tetramethylolmethane 6%, polyester bottles 13%, MALEIC ANHYDRIDE 2%, 2.8%, No. 200 solvent oil 45% of dimethylbenzene.
The preparation process of present embodiment is with embodiment 1, just increase rosin in the raw material, soya-bean oil, glycerine and rosin need be added in the reactor in the lump and heat up, after after the esterification insulation, when viscosity is 3.5-4.5s (Ge Shi pipe, 25 ℃), during acid value≤10mgKOH/g, cooling, latting drown, filtration, finished product.The Synolac that present embodiment makes is particularly suitable for being used for preparing ready mixed paint, rust-inhibiting paint and priming paint.
Embodiment 3, present embodiment adopt the following raw materials according proportioning by weight percentage: acidifying oil 20%, rosin 5%, tetramethylolmethane 6.5%, polyester bottles 15%, MALEIC ANHYDRIDE 1.2%, 2.8%, No. 200 solvent oil 45% of dimethylbenzene.
The preparation process of present embodiment does not just adopt glycerine in the raw material with embodiment 2, and adopts acidifying oil to replace soya-bean oil.The Synolac that present embodiment makes is particularly suitable for being used for preparing rust proof paint, has water tolerance and resistance to salt water preferably.
The Synolac that makes by the foregoing description all has special preservative property.After being made into iron oxide red anticorrosive paint, middle grey rust-inhibiting paint and iron oxide red primer, coat with lacquer respectively on the model, the above-mentioned lacquer made from former Synolac compares, and can obviously find out this effect.Its comparing result sees the following form:
Claims (7)
1. technology of utilizing waste polyester bottle to prepare Synolac, it is characterized in that using by weight percentage following proportion raw material, after esterification, finally make the Synolac finished product: oily 20-25%, polyvalent alcohol 5.5-8.2%, polyester bottles 13-15%, dimethylbenzene 2.5-3%, MALEIC ANHYDRIDE 1-2%, rosin 0-7%, 200# solvent oil 45-50%, wherein MALEIC ANHYDRIDE is used as catalyzer; Said oil is meant soya-bean oil or acidifying oil.
2. the technology of preparation Synolac as claimed in claim 1 is characterized in that also can adding in the reactant lithium hydroxide of 0.007-0.01% weight as antioxidant.
3. the technology of preparation Synolac as claimed in claim 1, it is characterized in that said polyvalent alcohol is tetramethylolmethane and/or glycerine, when selecting tetramethylolmethane for use separately, its weight percent is 6-7.5%, when the two is selected for use simultaneously, its weight percent is respectively: glycerine 1.0-1.6%, tetramethylolmethane 4.5-6.5%.
4. the technology of preparation Synolac as claimed in claim 3, it is characterized in that adopting and be prepared as follows step: in reaction vessel, add reactant oil and rosin, when rising to 220 ℃, temperature adds tetramethylolmethane afterwards, be warming up to 240 ℃ then, after alcoholysis is extremely clear, add polyester bottle slice when continuing to be warming up to 250 ℃, maintain the temperature at 250-260 ℃ of degraded after transparent, add MALEIC ANHYDRIDE when being cooled to 210 ℃, backflow dimethylbenzene, esterification insulation when being warming up to 230-240 ℃ then, esterification insulation Ge Shi pipe viscosity 3.5-10s to 25 ℃ of conditions, lower the temperature during acid value≤10mgKOH/g, resultant is added 200# solvent oil latting drown, promptly make the Synolac finished product behind the elimination waste residue.
5. the technology of preparation Synolac as claimed in claim 4 is characterized in that also comprising in the reactant glycerine.
6. the technology of preparation Synolac as claimed in claim 4 is characterized in that also can adding the antioxidant lithium hydroxide after the adding reactant tentatively heats up in the reaction vessel.
7. the technology of preparation Synolac as claimed in claim 6 adds the antioxidant lithium hydroxide when it is characterized in that being warming up to 120 ℃ behind the adding reactant in the reaction vessel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100160804A CN101585910B (en) | 2008-05-21 | 2008-05-21 | Process for preparing alkyd by using waste polyester bottle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100160804A CN101585910B (en) | 2008-05-21 | 2008-05-21 | Process for preparing alkyd by using waste polyester bottle |
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| Publication Number | Publication Date |
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| CN101585910A CN101585910A (en) | 2009-11-25 |
| CN101585910B true CN101585910B (en) | 2011-09-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2008100160804A Active CN101585910B (en) | 2008-05-21 | 2008-05-21 | Process for preparing alkyd by using waste polyester bottle |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845209B (en) * | 2010-05-11 | 2013-01-30 | 嘉宝莉化工集团股份有限公司 | Soybean oil modified alkyd as well as preparation method and application thereof in coating |
| CN102432851B (en) * | 2011-09-06 | 2014-11-05 | 天长市开林化工有限公司 | Liquid alkyd resin and preparation method thereof |
| CN103601877B (en) * | 2013-11-14 | 2015-09-30 | 新疆红山涂料有限公司 | High-solid alkyd resin and preparation method thereof |
| BR112016015467B1 (en) * | 2014-01-27 | 2021-05-11 | Swimc Llc | coating system and method, and, coated article |
| CN104479080B (en) * | 2014-12-31 | 2018-12-21 | 中昊北方涂料工业研究设计院有限公司 | A kind of water dispersible coatings prepared with pet waste and behenic acid |
| CN104530401A (en) * | 2015-01-05 | 2015-04-22 | 陕西源源化工有限责任公司 | Alkyd resin and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1090294A (en) * | 1993-10-18 | 1994-08-03 | 柳培溪 | A kind of manufacture method of terylene alkyd resin against weathering and ageing for paint |
| EP1245603A1 (en) * | 2001-03-30 | 2002-10-02 | Kansai Paint Co., Ltd. | Processes for producing aqueous alkyd resin dispersions |
| CN100999571A (en) * | 2007-01-12 | 2007-07-18 | 福建豪迪涂料科技股份有限公司 | Process of producing alkyd resin using waste dacron (polyester fibre) |
-
2008
- 2008-05-21 CN CN2008100160804A patent/CN101585910B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1090294A (en) * | 1993-10-18 | 1994-08-03 | 柳培溪 | A kind of manufacture method of terylene alkyd resin against weathering and ageing for paint |
| EP1245603A1 (en) * | 2001-03-30 | 2002-10-02 | Kansai Paint Co., Ltd. | Processes for producing aqueous alkyd resin dispersions |
| CN100999571A (en) * | 2007-01-12 | 2007-07-18 | 福建豪迪涂料科技股份有限公司 | Process of producing alkyd resin using waste dacron (polyester fibre) |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2002-128880A 2002.05.09 |
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