CN106398541A - Preparation method of rosin pentaerythritol ester for paint - Google Patents
Preparation method of rosin pentaerythritol ester for paint Download PDFInfo
- Publication number
- CN106398541A CN106398541A CN201610746480.5A CN201610746480A CN106398541A CN 106398541 A CN106398541 A CN 106398541A CN 201610746480 A CN201610746480 A CN 201610746480A CN 106398541 A CN106398541 A CN 106398541A
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- Prior art keywords
- weight
- paint
- rosin
- preparation
- temperature
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- 239000003973 paint Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 title abstract 6
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 title abstract 6
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 title abstract 6
- -1 pentaerythritol ester Chemical class 0.000 title abstract 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011787 zinc oxide Substances 0.000 claims abstract description 5
- VLTOSDJJTWPWLS-UHFFFAOYSA-N pent-2-ynal Chemical compound CCC#CC=O VLTOSDJJTWPWLS-UHFFFAOYSA-N 0.000 claims description 21
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 229910017052 cobalt Inorganic materials 0.000 claims description 10
- 239000010941 cobalt Substances 0.000 claims description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 10
- 229940059574 pentaerithrityl Drugs 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 6
- 238000005886 esterification reaction Methods 0.000 claims description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000010937 tungsten Substances 0.000 claims description 4
- 230000032050 esterification Effects 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 239000002253 acid Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract 2
- QVYYOKWPCQYKEY-UHFFFAOYSA-N [Fe].[Co] Chemical compound [Fe].[Co] QVYYOKWPCQYKEY-UHFFFAOYSA-N 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- DJOWTWWHMWQATC-KYHIUUMWSA-N Karpoxanthin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1(O)C(C)(C)CC(O)CC1(C)O)C=CC=C(/C)C=CC2=C(C)CC(O)CC2(C)C DJOWTWWHMWQATC-KYHIUUMWSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/04—Chemical modification, e.g. esterification
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
Relating to the technical field of deep processing of rosin, the invention discloses a preparation method of rosin pentaerythritol ester for paint. The method includes: adding rosin into a reaction kettle, introducing nitrogen, performing heating till rosin melting, lowering the temperature to 130DEG C-140DEG C, adding maleic anhydride to a first mixed solution, adjusting the temperature of the first mixed solution, conducting heat preservation for 2-2.5h, then adding pentaerythritol and 0.05-0.1 part by weight of a catalyst, conducting heating to 220DEG C-250DEG C, carrying out reaction until the iron cobalt color number of rosin pentaerythritol to less than or equal to 8.5, then stopping the reaction and nitrogen introduction, wherein the catalyst is tungstogermanic acid or zinc oxide. The product obtained by the method provided by the invention has the advantages of lighter color and high softening point.
Description
Technical field
The present invention relates to Colophonium deep process technology field, especially a kind of preparation side of paint pentalyn
Method.
Background technology
Pentalyn has outstanding heat-resisting, aging resistance and good stability, and the compatibility and dissolubility are good, good
Good surface resistivity and good color retention, therefore, pentalyn is usually used in the fields such as paint, ink, adhesive.
Pentalyn is applied to during paint it is desirable to its color is shallower, however, existing pentalyn often color is relatively
Deep, thus have impact on the outward appearance of paint.
Content of the invention
It is an object of the invention to provide a kind of preparation method of paint pentalyn, Colophonium season used by this paint
The preparation method of Doutrate can solve the saturate problem of pentalyn.
In order to solve the above problems, the technical solution used in the present invention is：
The preparation method of this paint pentalyn comprises the following steps：The Colophonium of 80～90 parts by weight is added
In reactor, it is passed through nitrogen, is heated to Colophonium fusing, reduce temperature to 130 DEG C～140 DEG C, add the horse of 2～4 parts by weight
Carry out anhydride, obtain the first mixed solution, to 180 DEG C～190 DEG C, insulation 2 hours～2.5 is little for the temperature of adjustment the first mixed solution
When, be subsequently adding the tetramethylolmethane of 10～13 parts by weight and the catalyst of 0.05～0.1 parts by weight, be warming up to 220 DEG C～
250 DEG C, stopped reaction during ferrum cobalt color number≤8.5 of esterification to Colophonium tetramethylolmethane, stop logical nitrogen；Wherein, catalyst
For tungsten germanic acid or zinc oxide.
In technique scheme, more specifically technical scheme can also be：Esterification reaction temperature is 230 DEG C～240 DEG C
Due to employing technique scheme, the present invention compared with prior art has the advantages that：
With the addition of in pentalyn preparation process of the present invention maleic anhydride be modified so that products obtained therefrom color relatively
Shallow, softening point is high, and when being painted using the pentalyn preparation of this method gained, drying varniss is fast, hardness of paint film, gloss
Has good, life-time service not yellowing.
Specific embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1
The preparation method of the present embodiment paint pentalyn is：The Colophonium of 80 parts by weight is added in reactor,
It is passed through nitrogen, is heated to Colophonium fusing, reduce temperature to 137 DEG C～140 DEG C, add the maleic anhydride of 2 parts by weight, obtain the
One mixed solution, the temperature of adjustment the first mixed solution, to 184 DEG C～186 DEG C, is incubated 2 hours, is subsequently adding 10 parts by weight
Tetramethylolmethane and 0.09 parts by weight catalyst, be warming up to 230 DEG C～235 DEG C, react 2 hours, detect Colophonium Ji Wusi
The ferrum cobalt color number of alcohol is 8.5, stopped reaction, stops logical nitrogen；Wherein, described catalyst is tungsten germanic acid.
The colour of the present embodiment pentalyn is 8.5（Ferrum cobalt method）, softening point（Ring and ball method）For 125 DEG C, acid number
（Milligrams per gram, in terms of KOH）For 13.6.
Embodiment 2
The preparation method of the present embodiment paint pentalyn is：The Colophonium of 85 parts by weight is added in reactor,
It is passed through nitrogen, is heated to Colophonium fusing, reduce temperature to 134 DEG C～138 DEG C, add the maleic anhydride of 3 parts by weight, obtain the
One mixed solution, the temperature of adjustment the first mixed solution, to 188 DEG C～190 DEG C, is incubated 2.5 hours, is subsequently adding 12 weight portions
The tetramethylolmethane of number and the catalyst of 0.075 parts by weight, are warming up to 237 DEG C～240 DEG C, react 2.5 hours, detect Colophonium season
The ferrum cobalt color number of penta tetrol is 8.2, stopped reaction, stops logical nitrogen；Wherein, described catalyst is zinc oxide.
The colour of the present embodiment pentalyn is 8.2（Ferrum cobalt method）, softening point（Ring and ball method）For 128 DEG C, acid number
（Milligrams per gram, in terms of KOH）For 15.3.
Embodiment 3
The preparation method of the present embodiment paint pentalyn is：The Colophonium of 84 parts by weight is added in reactor,
It is passed through nitrogen, is heated to Colophonium fusing, reduce temperature to 134 DEG C～137 DEG C, add the maleic anhydride of 4 parts by weight, obtain the
One mixed solution, the temperature of adjustment the first mixed solution, to 184 DEG C～187 DEG C, is incubated 2.3 hours, is subsequently adding 13 weight portions
The tetramethylolmethane of number and the catalyst of 0.1 parts by weight, are warming up to 220 DEG C～226 DEG C, react 3 hours, detect Colophonium Ji Wusi
The ferrum cobalt color number of alcohol is 7.8, stopped reaction, stops logical nitrogen；Wherein, described catalyst is zinc oxide.
The colour of the present embodiment pentalyn is 7.8（Ferrum cobalt method）, softening point（Ring and ball method）For 123 DEG C, acid number
（Milligrams per gram, in terms of KOH）For 12.7.
Embodiment 4
The preparation method of the present embodiment paint pentalyn is：The Colophonium of 90 parts by weight is added in reactor,
It is passed through nitrogen, is heated to Colophonium fusing, reduce temperature to 130 DEG C～132 DEG C, add the maleic anhydride of 2.5 parts by weight, obtain
First mixed solution, the temperature of adjustment the first mixed solution, to 180 DEG C～183 DEG C, is incubated 2.7 hours, is subsequently adding 12.5 weights
The amount tetramethylolmethane of number and the catalyst of 0.05 parts by weight, are warming up to 246 DEG C～250 DEG C, react 2.8 hours, detection pine
The ferrum cobalt color number of fragrant tetramethylolmethane is 8.4, stopped reaction, stops logical nitrogen；Wherein, described catalyst is tungsten germanic acid.
The colour of the present embodiment pentalyn is 8.4（Ferrum cobalt method）, softening point（Ring and ball method）For 129 DEG C, acid number
（Milligrams per gram, in terms of KOH）For 14.2.
Claims (2)
1. a kind of preparation method of paint pentalyn is it is characterised in that comprise the following steps：By 80～90 weight
The Colophonium of number adds in reactor, is passed through nitrogen, is heated to Colophonium fusing, reduces temperature to 130 DEG C～140 DEG C, add 2～
The maleic anhydride of 4 parts by weight, obtains the first mixed solution, and the temperature of adjustment the first mixed solution, to 180 DEG C～190 DEG C, is protected
Temperature 2 hours～2.5 hours, is subsequently adding the tetramethylolmethane of 10～13 parts by weight and the catalyst of 0.05～0.1 parts by weight,
It is warming up to 220 DEG C～250 DEG C, stopped reaction during ferrum cobalt color number≤8.5 of esterification to Colophonium tetramethylolmethane, stop logical nitrogen
Gas；Wherein, described catalyst is tungsten germanic acid or zinc oxide.
2. the preparation method of paint pentalyn according to claim 1 is it is characterised in that esterification temperature
Spend for 230 DEG C～240 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610746480.5A CN106398541A (en) | 2016-08-29 | 2016-08-29 | Preparation method of rosin pentaerythritol ester for paint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610746480.5A CN106398541A (en) | 2016-08-29 | 2016-08-29 | Preparation method of rosin pentaerythritol ester for paint |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106398541A true CN106398541A (en) | 2017-02-15 |
Family
ID=58003507
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610746480.5A Withdrawn CN106398541A (en) | 2016-08-29 | 2016-08-29 | Preparation method of rosin pentaerythritol ester for paint |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106398541A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110742298A (en) * | 2019-11-15 | 2020-02-04 | 湖北中烟工业有限责任公司 | Method for preventing tobacco sheets from being adhered during storage |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475776A (en) * | 2009-01-13 | 2009-07-08 | 中国林业科学研究院林产化学工业研究所 | Preparation of light colore high softening point maleated rosin pentaerythritol |
| CN102965024A (en) * | 2012-12-18 | 2013-03-13 | 普洱科茂林化有限公司 | Rosin viscosified resin as well as preparation method and application thereof |
| CN103436174A (en) * | 2013-08-27 | 2013-12-11 | 广西梧州松脂股份有限公司 | Preparation method of rosin glycerin ester |
| CN105038603A (en) * | 2015-07-31 | 2015-11-11 | 梧州市嘉盈树胶有限公司 | Method for preparing high-softening-point rosin glyceride |
| CN105802499A (en) * | 2016-04-15 | 2016-07-27 | 梧州市飞卓林产品实业有限公司 | Production method for polymerized rosin with softening point at 95 DEG C |
-
2016
- 2016-08-29 CN CN201610746480.5A patent/CN106398541A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475776A (en) * | 2009-01-13 | 2009-07-08 | 中国林业科学研究院林产化学工业研究所 | Preparation of light colore high softening point maleated rosin pentaerythritol |
| CN102965024A (en) * | 2012-12-18 | 2013-03-13 | 普洱科茂林化有限公司 | Rosin viscosified resin as well as preparation method and application thereof |
| CN103436174A (en) * | 2013-08-27 | 2013-12-11 | 广西梧州松脂股份有限公司 | Preparation method of rosin glycerin ester |
| CN105038603A (en) * | 2015-07-31 | 2015-11-11 | 梧州市嘉盈树胶有限公司 | Method for preparing high-softening-point rosin glyceride |
| CN105802499A (en) * | 2016-04-15 | 2016-07-27 | 梧州市飞卓林产品实业有限公司 | Production method for polymerized rosin with softening point at 95 DEG C |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110742298A (en) * | 2019-11-15 | 2020-02-04 | 湖北中烟工业有限责任公司 | Method for preventing tobacco sheets from being adhered during storage |
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| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20170215 |