CN106634615A - Preparation method of polymerized rosin pentaerythritol ester for paint - Google Patents
Preparation method of polymerized rosin pentaerythritol ester for paint Download PDFInfo
- Publication number
- CN106634615A CN106634615A CN201610747015.3A CN201610747015A CN106634615A CN 106634615 A CN106634615 A CN 106634615A CN 201610747015 A CN201610747015 A CN 201610747015A CN 106634615 A CN106634615 A CN 106634615A
- Authority
- CN
- China
- Prior art keywords
- hour
- newtrex
- pentaerythritol ester
- polymerized rosin
- catalyst
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- -1 pentaerythritol ester Chemical class 0.000 title claims abstract description 22
- 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 claims abstract description 11
- 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 claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 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 claims abstract description 11
- 239000003973 paint Substances 0.000 title abstract description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 20
- 235000011187 glycerol Nutrition 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims 1
- 235000011613 Pinus brutia Nutrition 0.000 claims 1
- 241000018646 Pinus brutia Species 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 claims 1
- 238000005886 esterification reaction Methods 0.000 abstract 1
- 125000005456 glyceride group Chemical group 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- VLTOSDJJTWPWLS-UHFFFAOYSA-N pent-2-ynal Chemical compound CCC#CC=O VLTOSDJJTWPWLS-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002904 solvent Substances 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
The invention discloses a preparation method of polymerized rosin pentaerythritol ester for paint, and relates to the technical field of deep processing of rosin. Polymerized rosin, pentaerythritol ester and a catalyst are added into a reaction vessel, heating is carried out, the polymerized rosin is melted and a reaction is carried out, heating is carried out sectionally, an esterification reaction is carried out till the polymerized rosin glyceride acid value (calculated by potassium hydroxide) is less than or equal to 17mg/g, and when the softening point is higher than or equal to 130 DEG C, the reaction stops. The softening point of the product is high than 130 DEG C.
Description
Technical field
The present invention relates to a kind of preparation of rosin deep process technology field, especially coating with newtrex pentaerythritol ester
Method.
Background technology
Newtrex pentaerythritol ester have than newtrex more resistant to oxidation, heat endurance more preferably, cohesive force it is higher, suitably
More characteristics such as solvent viscosity and extensive intermiscibility, dissolubility, also with more high softening-point, the features such as lower acid number,
It is widely used in adhesive, paint and the aspect such as ink and other polymer modification agents.Although newtrex pentaerythritol ester has
Numerous advantages, its softening point still has much room for improvement.
The content of the invention
It is an object of the invention to provide a kind of preparation method of coating with newtrex pentaerythritol ester, this coating is used poly-
Closing the preparation method of pentalyn can solve the problems, such as that softening point is low.
In order to solve the above problems, the technical solution used in the present invention is：This coating newtrex pentaerythritol ester
Preparation method be：Newtrex, pentaerythritol ester and catalyst are added into reactor, is stirred, heating makes newtrex
React in fusing, in the 1st hour, reactor temperature is increased to 180 DEG C～190 DEG C, the 2nd hour～the 2.5th hour, reacts
Temperature in the kettle rises to 200 DEG C～240 DEG C, and the 2.5th hour～the 3rd hour, reactor temperature was increased to 240 DEG C～250 DEG C, protected
Hold temperature-resistant, continue to react to polymerized rosin glycerol ester acid number (in terms of potassium hydroxide)≤10mg/g, and softening point >=130
DEG C when stop reaction；
Wherein, catalyst is zinc oxide or tungsten germanic acid；
The mass ratio of newtrex, glycerine and catalyst is 1：0.1～0.15：0.01～0.02.
In above-mentioned technical proposal, more specifically technical scheme can also be：
As a result of above-mentioned technical proposal, the present invention has the advantages that compared with prior art：
1st, the present invention makes newtrex react in fusing by heating, and reacting the heat for producing can also melt for newtrex
Energy is provided, the energy has been saved, production cost is reduced.
2nd, by way of progressively heating up, reaction condition is gentleer, carries out reacting balance for the present invention, reduces side reaction
Occur.
3rd, product softening point of the present invention is more than 130 DEG C.
Specific embodiment
With reference to embodiment, the invention will be further described：
Embodiment 1
The preparation method of the present embodiment coating newtrex pentaerythritol ester is：By newtrex, pentaerythritol ester and catalysis
Agent adds reactor, stirs, and heating makes newtrex react in fusing, and in the 1st hour, reactor temperature is increased to
183 DEG C～188 DEG C, the 2nd hour～the 2.5th hour, reactor temperature rose to 200 DEG C～207 DEG C, and the 2.5th hour～the 3rd is little
When, reactor temperature is increased to 240 DEG C～247 DEG C, and keeping temperature is constant, continues to react to polymerized rosin glycerol ester acid number
(being counted with potassium hydroxide) is as 16.4mg/g, and softening point stops reaction when being 133 DEG C；Catalyst is zinc oxide；
The mass ratio of newtrex, glycerine and catalyst is 1：0.1：0.01.
Embodiment 2
The preparation method of the present embodiment coating newtrex pentaerythritol ester is：By newtrex, pentaerythritol ester and catalysis
Agent adds reactor, stirs, and heating makes newtrex react in fusing, and in the 1st hour, reactor temperature is increased to
183 DEG C～190 DEG C, the 2nd hour～the 2.5th hour, reactor temperature rose to 227 DEG C～240 DEG C, and the 2.5th hour～the 3rd is little
When, reactor temperature is increased to 240 DEG C～246 DEG C, and keeping temperature is constant, continuation reaction to newtrex glycerine acid number (with
Potassium hydroxide meter) it is 16.2mg/g, and softening point stops reaction when being 136 DEG C；Catalyst is tungsten germanic acid；
The mass ratio of newtrex, glycerine and catalyst is 1：0.15：0.015.
Embodiment 3
The preparation method of the present embodiment coating newtrex pentaerythritol ester is：By newtrex, pentaerythritol ester and catalysis
Agent adds reactor, stirs, and heating makes newtrex react in fusing, and in the 1st hour, reactor temperature is increased to
180 DEG C～186 DEG C, the 2nd hour～the 2.5th hour, reactor temperature rose to 200 DEG C～212 DEG C, and the 2.5th hour～the 3rd is little
When, reactor temperature is increased to 243 DEG C～250 DEG C, and keeping temperature is constant, continues to react to polymerized rosin glycerol ester acid number
(being counted with potassium hydroxide) is as 15.8mg/g, and softening point stops reaction when being 136 DEG C；Catalyst is zinc oxide；
The mass ratio of newtrex, glycerine and catalyst is 1：0.13：0.02.
Claims (1)
1. a kind of coating preparation method of newtrex pentaerythritol ester, it is characterised in that comprise the following steps：Will polymerization pine
Fragrant, pentaerythritol ester and catalyst add reactor, stir, and heating makes newtrex react in fusing, the 1st hour
Interior, reactor temperature is increased to 180 DEG C～190 DEG C, the 2nd hour～the 2.5th hour, reactor temperature rise to 200 DEG C～
240 DEG C, the 2.5th hour～the 3rd hour, reactor temperature was increased to 240 DEG C～250 DEG C, and keeping temperature is constant, continued to react
To polymerized rosin glycerol ester acid number (in terms of potassium hydroxide)≤17mg/g, and stop reaction during softening point >=130 DEG C；
Wherein, the catalyst is zinc oxide or tungsten germanic acid；
The mass ratio of newtrex, glycerine and catalyst is 1：0.1～0.15：0.01～0.02.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610747015.3A CN106634615A (en) | 2016-08-29 | 2016-08-29 | Preparation method of polymerized rosin pentaerythritol ester for paint |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610747015.3A CN106634615A (en) | 2016-08-29 | 2016-08-29 | Preparation method of polymerized rosin pentaerythritol ester for paint |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106634615A true CN106634615A (en) | 2017-05-10 |
Family
ID=58852766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610747015.3A Withdrawn CN106634615A (en) | 2016-08-29 | 2016-08-29 | Preparation method of polymerized rosin pentaerythritol ester for paint |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106634615A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105860551A (en) * | 2016-05-12 | 2016-08-17 | 广西融水闽兴树脂有限公司 | Preparation method of rosin emulsion |
-
2016
- 2016-08-29 CN CN201610747015.3A patent/CN106634615A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105860551A (en) * | 2016-05-12 | 2016-08-17 | 广西融水闽兴树脂有限公司 | Preparation method of rosin emulsion |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for 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: 20170510 |