CN106010285A - Preparation method of disproportionated rosin - Google Patents
Preparation method of disproportionated rosin Download PDFInfo
- Publication number
- CN106010285A CN106010285A CN201610484493.XA CN201610484493A CN106010285A CN 106010285 A CN106010285 A CN 106010285A CN 201610484493 A CN201610484493 A CN 201610484493A CN 106010285 A CN106010285 A CN 106010285A
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- CN
- China
- Prior art keywords
- preparation
- disproportionated rosin
- passed
- rosin
- reaction
- 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.)
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- 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 30
- 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 30
- 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 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 150000001336 alkenes Chemical class 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011949 solid catalyst Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000011347 resin Substances 0.000 claims description 15
- 229920005989 resin Polymers 0.000 claims description 15
- 239000002808 molecular sieve Substances 0.000 claims description 14
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 14
- 238000007323 disproportionation reaction Methods 0.000 claims description 13
- 229910052756 noble gas Inorganic materials 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims description 5
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 5
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 208000011580 syndromic disease Diseases 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 4
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 4
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 6
- 239000007789 gas Substances 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- 239000011261 inert gas Substances 0.000 abstract 2
- 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 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000155 melt Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- QUUCYKKMFLJLFS-UHFFFAOYSA-N Dehydroabietan Natural products CC1(C)CCCC2(C)C3=CC=C(C(C)C)C=C3CCC21 QUUCYKKMFLJLFS-UHFFFAOYSA-N 0.000 description 1
- NFWKVWVWBFBAOV-UHFFFAOYSA-N Dehydroabietic acid Natural products OC(=O)C1(C)CCCC2(C)C3=CC=C(C(C)C)C=C3CCC21 NFWKVWVWBFBAOV-UHFFFAOYSA-N 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- NFWKVWVWBFBAOV-MISYRCLQSA-N dehydroabietic acid Chemical compound OC(=O)[C@]1(C)CCC[C@]2(C)C3=CC=C(C(C)C)C=C3CC[C@H]21 NFWKVWVWBFBAOV-MISYRCLQSA-N 0.000 description 1
- 229940118781 dehydroabietic acid Drugs 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber 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)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a preparation method of disproportionated rosin. The method particularly comprises the steps that refined rosin serves as the raw material and is added into a reaction kettle, inert gas is introduced into the reaction kettle, heating is conducted to 130 DEG C to 140 DEG C, and heating is conducted for 20 min to 30 min till the refined rosin is melted; introducing of the inert gas is stopped, 0.02-0.2 part of solid catalyst is added for a disproportionated reaction, in the reaction process, stirring is conducted ceaselessly, olefin gas is introduced, after the disproportionated reaction is finished, filtering is conducted to remove the catalyst, and the disproportionated rosin is obtained. According to the preparation method of the disproportionated rosin, the olefin gas is introduced, and crystallization resistance of the disproportionated rosin is improved.
Description
Technical field
The present invention relates to Colophonium deep process technology field, the preparation method of a kind of disproportionated rosin.
Background technology
Disproportionated rosin is in the presence of a catalyst, and by means of mineral acid and the effect of heat, the part making Colophonium is oxidized, and another part is reduced, and i.e. there occurs the product of dismutation reaction gained.Disproportionated rosin is dehydroabietic acid, dihydro rosin acid and the mixture of tetrahydrogenated rosin acid, and disproportionated rosin is relatively low due to production cost, is mainly used in synthetic rubber, ABS resin, water-soluble pressure-sensitive adhesive, printing-ink, organic pigment etc..
The preparation method of traditional disproportionated rosin is: add palladium-carbon catalyst after melted for Colophonium, dismutation reaction 3 hours～5 hours under the high temperature of 230 DEG C～290 DEG C, but the disproportionated rosin that the method produces relatively is easily generated crystallization, its transparency, dissolubility is made to reduce, fusing point raises, it is difficult to saponification, has the trend of recrystallization in a solvent, reduce use value.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of disproportionated rosin, this method can solve the problem that disproportionated rosin easily crystallizes.
In order to solve the problems referred to above, the technical solution used in the present invention is:
The preparation method of this disproportionated rosin is: with 10 parts～30 parts of resins as raw material, is added in reactor by described resin, is passed through noble gas, is heated to 130 DEG C～140 DEG C, heat 20 minutes～30 minutes in reactor, melted to resin；Stopping being passed through noble gas, add 0.02 part～0.2 part of solid catalyst carries out dismutation reaction, course of reaction is not stopped stirring and is passed through olefin gas, after dismutation reaction terminates, and Filtration of catalyst, i.e. obtain disproportionated rosin.
In technique scheme, more specifically technical scheme is it may also is that described alkene is propylene or butylene.
Further, described molecular sieve is to be prepared from kieselguhr for raw material.
Further, the preparation method of described molecular sieve is: after being calcined at 1200 DEG C～1250 DEG C by kieselguhr, add in the sodium hydroxide solution that substance withdrawl syndrome is 8mol/L, it is subsequently adding in sodium aluminate solution ageing, adding calcium chloride solution, arranging temperature is 80 DEG C, reacts 2 hours, the most cooled, wash, filter, be dried, obtain molecular sieve.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
1, the present invention is passed through olefin gas during dismutation reaction, improves the anti-crystallization of disproportionated rosin.
2, the present invention uses molecular sieve as catalyst, and activity is good, and chemical reaction rate is very fast.
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 disproportionated rosin is: with 10 parts of resins as raw material, is added in reactor by described resin, is passed through nitrogen, is heated to 130 DEG C, heat 20 minutes in reactor, melts to resin；Stopping logical nitrogen, add 0.2 part of molecular sieve catalyst and carry out dismutation reaction, course of reaction is not stopped stirring and is passed through butylene, after dismutation reaction terminates, and Filtration of catalyst, i.e. obtain disproportionated rosin.
The preparation method of the present embodiment molecular sieve is: after being calcined at 1200 DEG C～1210 DEG C by kieselguhr, add in the sodium hydroxide solution that substance withdrawl syndrome is 8mol/L, it is subsequently adding in sodium aluminate solution ageing, add calcium chloride solution, arranging temperature is 80 DEG C, react 2 hours, more cooled, wash, filter, be dried, obtain molecular sieve.
Embodiment 2
The preparation method of the present embodiment disproportionated rosin is: with 20 parts of resins as raw material, is added in reactor by described resin, is passed through noble gas, is heated to 135 DEG C, heat 25 minutes in reactor, melts to resin；Stopping being passed through noble gas, add 0.02 part of solid catalyst and carry out dismutation reaction, course of reaction is not stopped stirring and is passed through propylene, after dismutation reaction terminates, and Filtration of catalyst, i.e. obtain disproportionated rosin.
The preparation method of the present embodiment molecular sieve is: after being calcined at 1245 DEG C～1250 DEG C by kieselguhr, add in the sodium hydroxide solution that substance withdrawl syndrome is 8mol/L, it is subsequently adding in sodium aluminate solution ageing, add calcium chloride solution, arranging temperature is 80 DEG C, react 2 hours, more cooled, wash, filter, be dried, obtain molecular sieve.
Embodiment 3
The preparation method of the present embodiment disproportionated rosin is: with 30 parts of resins as raw material, is added in reactor by described resin, is passed through noble gas, is heated to 140 DEG C, heat 30 minutes in reactor, melts to resin；Stopping being passed through noble gas, add 0.1 part of solid catalyst and carry out dismutation reaction, course of reaction is not stopped stirring and is passed through propylene, after dismutation reaction terminates, and Filtration of catalyst, i.e. obtain disproportionated rosin.
The preparation method of the present embodiment molecular sieve is: after being calcined at 1230 DEG C～1237 DEG C by kieselguhr, add in the sodium hydroxide solution that substance withdrawl syndrome is 8mol/L, it is subsequently adding in sodium aluminate solution ageing, add calcium chloride solution, arranging temperature is 80 DEG C, react 2 hours, more cooled, wash, filter, be dried, obtain molecular sieve.
Claims (4)
1. the preparation method of a disproportionated rosin, it is characterised in that: with 10 parts～30 parts of resins as raw material, described resin is added in reactor, noble gas it is passed through in reactor, it is heated to 130 DEG C～140 DEG C, heats 20 minutes～30 minutes, melt to resin；Stopping being passed through noble gas, add 0.02 part～0.2 part of solid catalyst carries out dismutation reaction, course of reaction is not stopped stirring and is passed through olefin gas, after dismutation reaction terminates, and Filtration of catalyst, i.e. obtain disproportionated rosin.
The preparation method of disproportionated rosin the most according to claim 1, it is characterised in that described alkene is propylene or butylene.
The preparation method of disproportionated rosin the most according to claim 1 and 2, it is characterised in that described molecular sieve is to be prepared from kieselguhr for raw material.
The preparation method of disproportionated rosin the most according to claim 3, the preparation method that it is characterized in that described molecular sieve is: after being calcined at 1200 DEG C～1250 DEG C by kieselguhr, add in the sodium hydroxide solution that substance withdrawl syndrome is 8mol/L, it is subsequently adding in sodium aluminate solution ageing, adding calcium chloride solution, arranging temperature is 80 DEG C, reacts 2 hours, the most cooled, wash, filter, be dried, obtain molecular sieve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610484493.XA CN106010285A (en) | 2016-06-28 | 2016-06-28 | Preparation method of disproportionated rosin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610484493.XA CN106010285A (en) | 2016-06-28 | 2016-06-28 | Preparation method of disproportionated rosin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106010285A true CN106010285A (en) | 2016-10-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610484493.XA Pending CN106010285A (en) | 2016-06-28 | 2016-06-28 | Preparation method of disproportionated rosin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106010285A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113652171A (en) * | 2021-07-29 | 2021-11-16 | 广西大学 | Method for preparing disproportionated rosin with high dehydroabietic acid content |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436175A (en) * | 2013-08-27 | 2013-12-11 | 广西梧州松脂股份有限公司 | Method for increasing content of dehydroabietic acid in disproportionated rosin |
-
2016
- 2016-06-28 CN CN201610484493.XA patent/CN106010285A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436175A (en) * | 2013-08-27 | 2013-12-11 | 广西梧州松脂股份有限公司 | Method for increasing content of dehydroabietic acid in disproportionated rosin |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113652171A (en) * | 2021-07-29 | 2021-11-16 | 广西大学 | Method for preparing disproportionated rosin with high dehydroabietic acid content |
| CN113652171B (en) * | 2021-07-29 | 2022-12-06 | 广西大学 | Method for preparing disproportionated rosin with high dehydroabietic acid content |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161012 |