CN105907312A - Preparation method of pale rosin methyl ester - Google Patents
Preparation method of pale rosin methyl ester Download PDFInfo
- Publication number
- CN105907312A CN105907312A CN201610354026.5A CN201610354026A CN105907312A CN 105907312 A CN105907312 A CN 105907312A CN 201610354026 A CN201610354026 A CN 201610354026A CN 105907312 A CN105907312 A CN 105907312A
- Authority
- CN
- China
- Prior art keywords
- methyl ester
- preparation
- rosin methyl
- pale rosin
- distilling apparatus
- 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.)
- Pending
Links
- 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 24
- 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 23
- 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 23
- 150000004702 methyl esters Chemical class 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OVXRPXGVKBHGQO-UYWIDEMCSA-N methyl (1r,4ar,4br,10ar)-1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylate Chemical compound C1CC(C(C)C)=CC2=CC[C@H]3[C@@](C(=O)OC)(C)CCC[C@]3(C)[C@H]21 OVXRPXGVKBHGQO-UYWIDEMCSA-N 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 238000005292 vacuum distillation Methods 0.000 abstract 1
- 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 description 7
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000012790 confirmation Methods 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 230000002951 depilatory effect Effects 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- -1 fixastive Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 210000004761 scalp Anatomy 0.000 description 1
- 230000035943 smell Effects 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
- C09F1/02—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of pale rosin methyl ester, relating to the technical field of rosin deep processing. The method comprises the following steps: adding rosin methyl ester into a distilling apparatus, and inspecting the air tightness of the distilling apparatus; and after the air tightness of the distilling apparatus is perfect, vacuumizing to 50-250 pa, distilling, and collecting the fraction. The pale rosin methyl ester prepared by the vacuum distillation method can remove most impurities in the rosin methyl ester. The obtained product has the advantages of low cost, favorable properties and wider applicability.
Description
Technical field
The present invention relates to Colophonium deep process technology field, the preparation method of a kind of pale rosin methyl ester.
Background technology
Colophonium is the Renewable resource of China's abundant, and annual production reaches more than 60 ten thousand tons, ranks first in the world.Colophonium processization
Learn modification and can obtain a series of deep processed product, the every field being widely applied in daily life, these deep processed products
Value ratio raw material Colophonium improve decades of times.
Abalyn is a kind of Colophonium deep processed product being in a liquid state at normal temperatures, by Colophonium with methanol in certain temperature
Prepare with carrying out esterification under pressure condition.Due to the application performance that itself is excellent, abalyn can be used as surface and lives
Property agent, viscosifier are applied to plastics, rubber, coating and gluing industry.
Along with the further development of science and technology, the application of abalyn is also continuously available expansion: abalyn can conduct
Lasting agent is applied to the production of essence, perfume and depilatory cream, is applied to sensitive material, metal as solvent resistant and anti-chemical coating
Preparation with plastics；The production of binder, plaster and scalp pomade it is applied to as chemical addition agent；It is alternatively arranged as microscopical immersion oil agent
And food fixastive and food additive.But, these products are more and more higher to the prescription of abalyn, especially should
When the health grade product such as depilatory cream, fixastive, food additive, it is desirable to it possesses lighter color, higher purity
And relatively low abnormal smells from the patient.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of pale rosin methyl ester, this preparation method can solve Colophonium
The problem that methyl ester product colour is deeper.
In order to solve the problems referred to above, the technical solution used in the present invention is:
The preparation method of this pale rosin methyl ester is: added by abalyn in distilling apparatus, checks the airtight of distilling apparatus
Property, after confirming that device air-tightness is intact, it is evacuated to 50 handkerchiefs～250 handkerchiefs, is heated to 212 DEG C～220 DEG C, be incubated distillation 1
Hour～2 hours, collect fraction, i.e. obtain pale rosin methyl ester product.
In technique scheme, more specifically technical scheme is it may also is that the rotating speed of distilling apparatus is 20 revs/min～60
Rev/min.
Further, after abalyn is added distilling apparatus, connect receiving flask, vacuum tube, open condensate cooler
Cooling water, then adjusts alembic rotating speed, can carry out air-leakage test after evacuation.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
1, the present invention uses the method for vacuum distilling to prepare pale rosin methyl ester fat, and the method can remove in abalyn does not joins
With the rosin resin acid monomers being esterified, neutral substance etc., products obtained therefrom is of light color, acid number is low, purity is high, viscosity is bigger.
2, the inventive method technique is simple, and production cost is relatively low.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The preparation method of the present embodiment pale rosin methyl ester is: is put in 5L revolving bottle by 2500 grams of abalyns, connects and connect
By bottle and with vacuum inspection, confirm system air-tightness intact.Distallation systm is evacuated to 50Pa, checks confirmation system air-tightness
After intact, beginning to warm up distillation, by room temperature to 212 DEG C～220 DEG C, insulation distillation 1 hour, stop distillation, this fraction is i.e.
For pale rosin methyl ester.
The present embodiment pale rosin methyl ester is pale yellow transparent thick liquid, acid number 2.2mg/g, color 1(ferrum cobalt color), viscous
Degree (25 DEG C) is 3500mp.
Embodiment 2
The preparation method of the present embodiment pale rosin methyl ester is: is put in 5L revolving bottle by 2500 grams of abalyns, connects and connect
By bottle and with vacuum inspection, confirm system air-tightness intact.Distallation systm is evacuated to 200Pa, checks that confirmation system is airtight
Property intact after, begin to warm up distillation, by room temperature to 212 DEG C～220 DEG C, insulation distillation 1.5 hours, stop distillation, this evaporates
Divide and be pale rosin methyl ester.
The present embodiment pale rosin methyl ester pale yellow transparent thick liquid, acid number 2.1mg/g, color 1-(ferrum cobalt color), viscous
Degree (25 DEG C) is 3450mp.s.
Claims (3)
1. the preparation method of a pale rosin methyl ester, it is characterised in that preparation process is: abalyn is added distilling apparatus
In, open vacuum the air-tightness of rotary distillation bottle is detected, confirm device air-tightness intact after, be evacuated to 50 handkerchiefs～
250 handkerchiefs, are heated to 212 DEG C～220 DEG C, insulation distillation 1 hour～2 hours, collect fraction, i.e. obtain pale rosin methyl ester
Product.
The preparation method of pale rosin methyl ester the most according to claim 1, it is characterised in that: the rotating speed of described distilling apparatus
It it is 20 revs/min～60 revs/min.
The preparation method of pale rosin methyl ester the most according to claim 1 and 2, it is characterised in that: abalyn is added
After distilling apparatus, connect receiving flask, vacuum tube, open condensate cooler cooling water, then adjust alembic rotating speed, evacuation
After can carry out air-leakage test.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610354026.5A CN105907312A (en) | 2016-05-25 | 2016-05-25 | Preparation method of pale rosin methyl ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610354026.5A CN105907312A (en) | 2016-05-25 | 2016-05-25 | Preparation method of pale rosin methyl ester |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105907312A true CN105907312A (en) | 2016-08-31 |
Family
ID=56741404
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610354026.5A Pending CN105907312A (en) | 2016-05-25 | 2016-05-25 | Preparation method of pale rosin methyl ester |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105907312A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573851A (en) * | 2017-09-18 | 2018-01-12 | 广西众昌树脂有限公司 | The processing method of abalyn |
| CN110760266A (en) * | 2019-08-12 | 2020-02-07 | 德庆华彩合成树脂有限公司 | Water-soluble fumaric acid modified rosin resin and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007092250A2 (en) * | 2006-02-02 | 2007-08-16 | Hexion Specialty Chemicals Inc. | Rosin ester with low color and process for preparing same |
| CN103627325A (en) * | 2013-11-28 | 2014-03-12 | 广东科茂林产化工股份有限公司 | Preparation method of light-colored low-odor tall oil rosin ester |
| CN104087180A (en) * | 2014-07-30 | 2014-10-08 | 广西众昌树脂有限公司 | Preparation method of pale rosin ester |
| CN104559793A (en) * | 2013-12-07 | 2015-04-29 | 广西梧州日成林产化工股份有限公司 | High-vacuum continuous distillation production method of light-colored rosin |
-
2016
- 2016-05-25 CN CN201610354026.5A patent/CN105907312A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007092250A2 (en) * | 2006-02-02 | 2007-08-16 | Hexion Specialty Chemicals Inc. | Rosin ester with low color and process for preparing same |
| CN103627325A (en) * | 2013-11-28 | 2014-03-12 | 广东科茂林产化工股份有限公司 | Preparation method of light-colored low-odor tall oil rosin ester |
| CN104559793A (en) * | 2013-12-07 | 2015-04-29 | 广西梧州日成林产化工股份有限公司 | High-vacuum continuous distillation production method of light-colored rosin |
| CN104087180A (en) * | 2014-07-30 | 2014-10-08 | 广西众昌树脂有限公司 | Preparation method of pale rosin ester |
Non-Patent Citations (3)
| Title |
|---|
| 吴春华等: "浅色松香酯的研究进展", 《四川林业科技》 * |
| 潘长华: "《实用小化工生产大全 第2卷 林化制品•农化制品•生化制品•天然色素•有机中间体•涂料》", 31 December 1997 * |
| 高德华等: "浅色松香酯制造工艺研究中试报告", 《林产化学与工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107573851A (en) * | 2017-09-18 | 2018-01-12 | 广西众昌树脂有限公司 | The processing method of abalyn |
| CN110760266A (en) * | 2019-08-12 | 2020-02-07 | 德庆华彩合成树脂有限公司 | Water-soluble fumaric acid modified rosin resin and preparation method thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160831 |