CN104448266A - Terminal hydroxyl polyester resin for co-extrusion extinction powder coating and preparation method of terminal hydroxyl polyester resin - Google Patents
Terminal hydroxyl polyester resin for co-extrusion extinction powder coating and preparation method of terminal hydroxyl polyester resin Download PDFInfo
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 title claims abstract description 61
- 239000000843 powder Substances 0.000 title claims abstract description 38
- 238000000576 coating method Methods 0.000 title claims abstract description 36
- 239000011248 coating agent Substances 0.000 title claims abstract description 35
- 229920001225 polyester resin Polymers 0.000 title claims abstract description 33
- 239000004645 polyester resin Substances 0.000 title claims abstract description 33
- 230000008033 biological extinction Effects 0.000 title claims abstract description 28
- 238000001125 extrusion Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000032050 esterification Effects 0.000 claims abstract description 19
- 238000005886 esterification reaction Methods 0.000 claims abstract description 19
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims abstract description 10
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 6
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 21
- 239000002253 acid Substances 0.000 claims description 20
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 239000003112 inhibitor Substances 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- NPAIMXWXWPJRES-UHFFFAOYSA-N butyltin(3+) Chemical compound CCCC[Sn+3] NPAIMXWXWPJRES-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 3
- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims description 2
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 2
- 230000009477 glass transition Effects 0.000 abstract 1
- 239000002932 luster Substances 0.000 abstract 1
- 229920005989 resin Polymers 0.000 description 15
- 239000011347 resin Substances 0.000 description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 10
- 238000001816 cooling Methods 0.000 description 7
- 238000012423 maintenance Methods 0.000 description 6
- 150000003504 terephthalic acids Chemical class 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000006085 branching agent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 235000021168 barbecue Nutrition 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 235000013847 iso-butane Nutrition 0.000 description 1
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229940059574 pentaerithrityl Drugs 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N sec-butylidene Natural products CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Landscapes
- Polyesters Or Polycarbonates (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses terminal hydroxyl polyester resin for co-extrusion extinction powder coating and a preparation method of the terminal hydroxyl polyester resin. The terminal hydroxyl polyester resin comprises trimethylolpropane, terephthalic acid, isophthalic acid, neopentyl glycol, an antioxygen and an esterification catalyst. Compared with the prior art, the synthesized polyester resin has the advantages that the glass transition temperature Tg of the polyester resin is higher than 51 DEG C; the polyester resin can provide a good storage stability; the viscosity is 2800-3000mPa.s (200 DEG C), and a good leveling effect can be provided due to the low viscosity; the polyester resin has a high hydroxyl value, carries out co-extrusion extinction with a low hydroxyl value, and has low luster being 7-10 percent.
Description
Technical field
The present invention relates to art of powder coatings, be specifically related to a kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin and preparation method thereof.
Background technology
Along with the fast development of powder coating industry, Flat paint all has a wide range of applications in decoration and building.And powder coating extinction method has multiple: the mode 1, by adding physics or chemical quenching agent realizes delustring; 2, being dry mixed rear spraying by weight 1:1 after adopting two kinds of active resins to make powder respectively utilizes the difference of two curing components rates to realize delustring, does not need to add any matting agent and can obtain low gloss; 3, jointly to be extruded by weight proportioning by two kinds of resins and solidifying agent and make powder spraying, can be made into the Flat paint of more low gloss.
When adopting the second technology, require very high to the reactive resin used, first, increase the difficulty in producing, the bad control of stability of product, secondly, pulverizing process step increases, increase cost, externality factor also increases, and as adopted the third method, not only can save time, also can reduce production cost, be following development trend simultaneously.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprising following composition by weight:
Described branching agent is one or more in TriMethylolPropane(TMP), trimethylolethane, tetramethylolmethane.
Described dibasic alcohol is BDO, one or more in 1,4 cyclohexane dimethanol, neopentyl glycol.
Described oxidation inhibitor is one or both in tributyl phosphate, triphenyl phosphite.
Described esterifying catalyst is one or both in Mono-n-butyltin, Dibutyltin oxide.
Further, a kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises following composition by weight:
The preparation method of a kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin provided by the invention, comprises the following steps:
A, esterification step: in building-up reactions container, the branching agent dropping into 0 ~ 0.4 part of dibasic alcohol and 9.6 ~ 10.2 parts is heated to material melting, then under agitation terephthalic acid 1 ~ 3 part and m-phthalic acid 7 ~ 9 parts and 0.02 ~ 0.03 part of esterifying catalyst is dropped into, after envelope still in nitrogen atmosphere progressively reacting by heating, generate to without overhead product, the acid number of reactant is 3 ~ 6mgKOH/g;
B, vacuum process: in the reactant that esterification step obtains, add 0.02 ~ 0.03 part of oxidation inhibitor, be cooled to 190 ~ 210 DEG C, vacuum tightness for-0.096mpa time react, until reactant reaches acid number 0.5 ~ 3mgKOH/g, viscosity 2800-3000mPa.s (200 DEG C) and hydroxyl value 280 ~ 320mgKOH/g, i.e. obtained crowded extinction powder coating hydroxyl telechelic polyester resin.
Be heated to material melting described in step a, Heating temperature is 50 ~ 100 DEG C.
Reacting by heating described in step a, temperature is 230 ~ 240 DEG C.
Further, the preparation method of a kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin provided by the invention, comprises the following steps:
A, esterification step: in building-up reactions container, drop into neopentyl glycol 0 ~ 0.4 part and three hydroxyls
Methylpropane 9.6 ~ 10.2 parts is heated to material melting, then under agitation drops into benzene two
1 ~ 3 part, formic acid and m-phthalic acid 7 ~ 9 parts and 0.02 ~ 0.03 part of esterifying catalyst, envelope
After still in nitrogen atmosphere progressively reacting by heating, to without overhead product generation, the acid of reactant
Value is 3 ~ 6mgKOH/g;
B, vacuum process: in the reactant that esterification step obtains, add 0.02 ~ 0.03 part of oxidation inhibitor, be cooled to 190 ~ 210 DEG C, vacuum tightness for-0.096mpa time react, until reactant reaches acid number 0.5 ~ 3mgKOH/g, viscosity 2800-3000mPa.s (200 DEG C) and hydroxyl value 280 ~ 320mgKOH/g, i.e. obtained crowded extinction powder coating hydroxyl telechelic polyester resin.
Be heated to material melting described in step a, Heating temperature is 50 ~ 100 DEG C.
Reacting by heating described in step a, temperature is 230 ~ 240 DEG C.
Compare with prior art, the vibrin of the present invention's synthesis has the following advantages: the second-order transition temperature Tg>51 DEG C of vibrin, can provide good stability in storage; Viscosity 2800-3000mPa.s (200 DEG C), viscosity low energy provides good levelling effect; Have higher hydroxyl value, with the delustring of low hydroxyl value co-extrusion, having very low gloss is 7-10%.
Dibasic alcohol used in formula is neopentyl glycol, the polyester product of its synthesis has the performance of excellent chemical stability, weathering resistance, thermostability and UV resistant irradiation, used branching agent is TriMethylolPropane(TMP) is a kind of trivalent alcohol, and it has the soundness, erosion resistance, the stopping property that improve resin; Satisfactory stability is had for hydrolysis and oxidation.Added terephthalic acid and m-phthalic acid are package stability in order to increase synthetic resins and weathering resistance on the one hand, also reduce the activity of resin on the other hand, are easy to produce.In a word while guarantee low gloss levelling is good, improve package stability and the weathering resistance of resin as far as possible.
Specific implementation method
Embodiment 1
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the component of following weight part:
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the following steps:
A, esterification step: in building-up reactions container, input newly defends glycol 0.2 part and TriMethylolPropane(TMP) 9.9 parts is heated to material melting, Heating temperature is 80 DEG C, then under agitation 8.8 parts of m-phthalic acids, 1.2 parts of terephthalic acids and 0.02 part of Mono-n-butyltin are dropped into, after envelope still in nitrogen atmosphere progressively reacting by heating, slowly be warming up to 230 DEG C of maintenances, till generating without overhead product, now the acid number of reactant is 4.6mgKOH/g;
B, vacuum process: the triphenyl phosphite oxidation inhibitor adding 0.02 part in the reactant that esterification step obtains, cooling is 190 DEG C, vacuum tightness is reacted for during-0.096mpa, now acid number AV=2.6mgKOH/g, the viscosity η=2800mPa.s (200 DEG C) of reactant and hydroxyl value HV=310mgKOH/g.
Embodiment 2
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the component of following weight part:
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the following steps:
A, esterification step: in building-up reactions container, input newly defends glycol 0.12 part and TriMethylolPropane(TMP) 10.0 parts is heated to material melting, Heating temperature is 70 DEG C, then under agitation 7.6 parts of m-phthalic acids, 2.5 parts of terephthalic acids and 0.026 part of Mono-n-butyltin are dropped into, after envelope still in nitrogen atmosphere progressively reacting by heating, slowly be warming up to 235 DEG C of maintenances, till generating without overhead product, now the acid number of reactant is 4.3mgKOH/g;
B, vacuum process: the triphenyl phosphite oxidation inhibitor adding 0.026 part in the reactant that esterification step obtains, cooling is 210 DEG C, vacuum tightness is reacted for during-0.096mpa, now acid number AV=2.0mgKOH/g, the viscosity η=2860mPa.s (200 DEG C) of reactant and hydroxyl value HV=305mgKOH/g.
Embodiment 3
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the component of following weight part:
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the following steps:
A, esterification step: in building-up reactions container, drop into TriMethylolPropane(TMP) 10.1 parts and be heated to material melting, Heating temperature is 90 DEG C, then under agitation 8 parts of m-phthalic acids, 2 parts of terephthalic acids and 0.023 part of Mono-n-butyltin are dropped into, after envelope still in nitrogen atmosphere progressively reacting by heating, slowly be warming up to 235 DEG C of maintenances, till generating without overhead product, now the acid number of reactant is 4.0mgKOH/g;
B, vacuum process: the triphenyl phosphite oxidation inhibitor adding 0.023 part in the reactant that esterification step obtains, cooling is 200 DEG C, vacuum tightness is reacted for during-0.096mpa, now acid number AV=1.7mgKOH/g, the viscosity η=2960mPa.s (200 DEG C) of reactant and hydroxyl value HV=300mgKOH/g.
Embodiment 4
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the component of following weight part:
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the following steps:
A, esterification step: in building-up reactions container, input newly defends glycol 0.3 part and TriMethylolPropane(TMP) 9.9 parts is heated to material melting, Heating temperature is 65 DEG C, then under agitation 8.4 parts of m-phthalic acids, 1.8 parts of terephthalic acids and 0.022 part of Mono-n-butyltin are dropped into, after envelope still in nitrogen atmosphere progressively reacting by heating, slowly be warming up to 230 ~ 235 DEG C of maintenances, till generating without overhead product, now the acid number of reactant is 3.6mgKOH/g;
B, vacuum process: the triphenyl phosphite oxidation inhibitor adding 0.023 part in the reactant that esterification step obtains, cooling is 210 DEG C, vacuum tightness is reacted for during-0.096mpa, now acid number AV=1.5mgKOH/g, the viscosity η=2980mPa.s (200 DEG C) of reactant and hydroxyl value HV=296mgKOH/g.
Embodiment 5
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the component of following weight part:
A kind of co-extrusion extinction powder coating hydroxyl telechelic polyester resin, comprises the following steps:
A, esterification step: in building-up reactions container, input newly defends glycol 0.4 part and TriMethylolPropane(TMP) 9.65 parts is heated to material melting, Heating temperature is 100 DEG C, then under agitation 7.25 parts of m-phthalic acids, 2.95 parts of terephthalic acids and 0.022 part of Mono-n-butyltin are dropped into, after envelope still in nitrogen atmosphere progressively reacting by heating, slowly be warming up to 230 ~ 240 DEG C of maintenances, till generating without overhead product, now the acid number of reactant is 4.6mgKOH/g;
B, vacuum process: the triphenyl phosphite oxidation inhibitor adding 0.023 part in the reactant that esterification step obtains, cooling is 210 DEG C, vacuum tightness is reacted for during-0.096mpa, now acid number AV=1.8mgKOH/g, the viscosity η=2990mPa.s (200 DEG C) of reactant and hydroxyl value HV=293mgKOH/g.
A kind of preparation method of low hydroxyl value resin B:
A, esterification step: in building-up reactions container, input newly defends glycol 8 parts and TriMethylolPropane(TMP) 0.3 part is heated to material melting, Heating temperature is 50 ~ 100 DEG C, then under agitation 9.6 parts of m-phthalic acids, 2 parts of terephthalic acids and 0.02 part of Mono-n-butyltin are dropped into, after envelope still in nitrogen atmosphere progressively reacting by heating, slowly be warming up to 240 DEG C of maintenances, till generating without overhead product, now the acid number of reactant is 10.1mgKOH/g;
B, vacuum process: the triphenyl phosphite oxidation inhibitor adding 0.02 part in the reactant that esterification step obtains, cooling is 220 DEG C, vacuum tightness is reacted for during-0.096mpa, now acid number AV=0.8mgKOH/g, the viscosity η=5550mPa.s (200 DEG C) of reactant and hydroxyl value HV=46mgKOH/g;
After c, vacuum process terminate, when cooling to 200 DEG C, the dibutyl tin laurate adding 0.01 part maintains 20min, obtains low hydroxyl value resin B.
The performance of high hydroxyl Resin A prepared by embodiment of the present invention 1-5 and low hydroxyl value resin B is embodied by should be used in powder coating.The high hydroxyl Resin A that in powder coating prepared by embodiment of the present invention 1-5 and low hydroxyl value resin B 1:3 by weight ratio, solidifying agent is masked isocyanate 1530-B, and its pigment is titanium dioxide, filler is ultra-fine barium and conventional additives is flow agent, st-yrax, wetting enhancer 701.The formula of powder coating is as following table 1
The preparation flow of powder coating:
Sample: accurately sample by above-mentioned formula.
Pre-mixing: fully shake up in the plastics bag of cleaning.
Extrude compressing tablet: be that 30rpm extrudes and compressing tablet with screw speed in Yantai Ling Yu twin screw experiment forcing machine (SLJ-40).
Powder process: sheet stock grinds in coffee grinder, 200 eye mesh screens sieve.
Spraying: spray under the manual electrostatic gun of 40 kilovolts respectively, coating materials is iron plate.
Barbecue: at 200 DEG C of barbecue 10min
Table 1
The embodiment label of the vibrin of the part indicating embodiment in table 1 to be also the present invention be synthesis, above-mentioned mass unit is: gram.
Embodiment 1 ' high hydroxyl Resin A used is prepared by embodiment 1, and embodiment 2 ' high hydroxyl Resin A used is prepared by embodiment 2, and embodiment 3 ' high hydroxyl Resin A used is prepared by embodiment 3,
Embodiment 4 ' high hydroxyl Resin A used is prepared by embodiment 4, and embodiment 5 ' high hydroxyl Resin A used is prepared by embodiment 5.
It is 9.0mgKOH/g. hydroxyl value is 286mgKOH/g that resin C in table 1 tests acid number as a comparison, and be refreshing sword high hydroxyl value resin, it is 6.0mgKOH/g that resin D tests acid number as a comparison, and hydroxyl value is 283mgKOH/g, is Mai Tugao hydroxyl resin.Ultra-fine barium is Qingdao east wind, and titanium dioxide is Sichuan dragon boa, and flow agent, st-yrax, 701 are South Sea chemistry.
The performance test results is as shown in table 2
Table 2
From table 1,2, high hydroxyl Resin A prepared by the inventive method and low hydroxyl value resin co-extrusion can obtain lower extinction powder coating, gloss <10%.The powder coating gloss that the vibrin utilizing us to synthesize and co-extrusion method obtain than conventional high hydroxyl resin-made is low by more than 10%; The obtained smooth exquisiteness of powder coating solidification film, has fine appearance of film, has very low gloss and have certain weathering resistance simultaneously.
Claims (6)
1. a co-extrusion extinction powder coating hydroxyl telechelic polyester resin, is characterized in that, described hydroxyl telechelic polyester resin comprises following composition by weight:
2. co-extrusion extinction powder coating hydroxyl telechelic polyester resin according to claim 1, is characterized in that, described oxidation inhibitor is one or both in tributyl phosphate, triphenyl phosphite.
3. co-extrusion extinction powder coating hydroxyl telechelic polyester resin according to claim 1, is characterized in that, described esterifying catalyst is one or both in Mono-n-butyltin, Dibutyltin oxide.
4. a preparation method for co-extrusion extinction powder coating hydroxyl telechelic polyester resin according to claim 1, it is characterized in that, described preparation method comprises the following steps:
A, esterification step: in building-up reactions container, drop into neopentyl glycol 0 ~ 0.4 part and be heated to material melting with TriMethylolPropane(TMP) 9.6 ~ 10.2 parts, then under agitation terephthalic acid 1 ~ 3 part and m-phthalic acid 7 ~ 9 parts and 0.02 ~ 0.03 part of esterifying catalyst is dropped into, after envelope still in nitrogen atmosphere progressively reacting by heating, generate to without overhead product, the acid number of reactant is 3 ~ 6mgKOH/g;
B, vacuum process: in the reactant that esterification step obtains, add 0.02 ~ 0.03 part of oxidation inhibitor, be cooled to 190 ~ 210 DEG C, vacuum tightness for-0.096mpa time react, until reactant reaches acid number 0.5 ~ 3mgKOH/g, viscosity 2800-3000mPa.s (200 DEG C) and hydroxyl value 280 ~ 320mgKOH/g, i.e. obtained crowded extinction powder coating hydroxyl telechelic polyester resin.
5. preparation method according to claim 4, is characterized in that, is heated to material melting described in step a, and Heating temperature is 50 ~ 100 DEG C.
6. preparation method according to claim 4, is characterized in that, reacting by heating described in step a, and temperature is 230 ~ 240 DEG C.
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| CN201410692150.3A CN104448266A (en) | 2014-11-25 | 2014-11-25 | Terminal hydroxyl polyester resin for co-extrusion extinction powder coating and preparation method of terminal hydroxyl polyester resin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254863A (en) * | 2015-10-31 | 2016-01-20 | 安徽神剑新材料股份有限公司 | Mixed polyester resin and preparation method and powder coating thereof |
| CN112409908A (en) * | 2020-10-11 | 2021-02-26 | 芜湖市森沐知识产权科技服务有限公司 | Polyurethane extinction powder coating and synthesis method thereof |
| CN112552497A (en) * | 2020-12-10 | 2021-03-26 | 黄山正杰新材料有限公司 | High-hydroxyl-value polyester resin for extinction type powder coating and preparation method and application thereof |
| CN113429550A (en) * | 2021-08-16 | 2021-09-24 | 安徽神剑新材料股份有限公司 | Polyester resin for detergent powder-resistant paint and preparation method and application thereof |
| CN114349942A (en) * | 2021-12-13 | 2022-04-15 | 安徽神剑新材料股份有限公司 | Bifunctional polyester resin, preparation method thereof and extinction powder coating |
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| CN105254863A (en) * | 2015-10-31 | 2016-01-20 | 安徽神剑新材料股份有限公司 | Mixed polyester resin and preparation method and powder coating thereof |
| CN105254863B (en) * | 2015-10-31 | 2017-08-29 | 安徽神剑新材料股份有限公司 | A kind of mixed polyester resin and preparation method thereof, powdery paints |
| CN112409908A (en) * | 2020-10-11 | 2021-02-26 | 芜湖市森沐知识产权科技服务有限公司 | Polyurethane extinction powder coating and synthesis method thereof |
| CN112552497A (en) * | 2020-12-10 | 2021-03-26 | 黄山正杰新材料有限公司 | High-hydroxyl-value polyester resin for extinction type powder coating and preparation method and application thereof |
| CN113429550A (en) * | 2021-08-16 | 2021-09-24 | 安徽神剑新材料股份有限公司 | Polyester resin for detergent powder-resistant paint and preparation method and application thereof |
| CN114349942A (en) * | 2021-12-13 | 2022-04-15 | 安徽神剑新材料股份有限公司 | Bifunctional polyester resin, preparation method thereof and extinction powder coating |
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