CN106010273A - Method for preparing light-color disproportionated rosin by using phosphoric acid compound ceramsite decolorising agent - Google Patents
Method for preparing light-color disproportionated rosin by using phosphoric acid compound ceramsite decolorising agent Download PDFInfo
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- CN106010273A CN106010273A CN201610385125.XA CN201610385125A CN106010273A CN 106010273 A CN106010273 A CN 106010273A CN 201610385125 A CN201610385125 A CN 201610385125A CN 106010273 A CN106010273 A CN 106010273A
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- phosphoric acid
- disproportionated rosin
- method preparing
- decolorising agent
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000000034 method Methods 0.000 title claims abstract description 52
- 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 51
- 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 48
- 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 48
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 46
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 27
- -1 phosphoric acid compound Chemical class 0.000 title abstract description 5
- 239000007788 liquid Substances 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 12
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005352 clarification Methods 0.000 claims abstract description 6
- 238000004062 sedimentation Methods 0.000 claims abstract description 5
- 239000000919 ceramic Substances 0.000 claims abstract description 4
- 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 28
- 239000002131 composite material Substances 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 8
- 235000013877 carbamide Nutrition 0.000 claims description 8
- 238000007323 disproportionation reaction Methods 0.000 claims description 8
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 230000006835 compression Effects 0.000 claims description 4
- 238000007906 compression Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 238000004299 exfoliation Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 2
- 239000000047 product Substances 0.000 abstract description 13
- 239000002253 acid Substances 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000004519 grease Substances 0.000 abstract 4
- 239000007795 chemical reaction product Substances 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- BTXXTMOWISPQSJ-UHFFFAOYSA-N 4,4,4-trifluorobutan-2-one Chemical compound CC(=O)CC(F)(F)F BTXXTMOWISPQSJ-UHFFFAOYSA-N 0.000 description 3
- BQACOLQNOUYJCE-FYZZASKESA-N Abietic acid Natural products CC(C)C1=CC2=CC[C@]3(C)[C@](C)(CCC[C@@]3(C)C(=O)O)[C@H]2CC1 BQACOLQNOUYJCE-FYZZASKESA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 2
- 235000011613 Pinus brutia Nutrition 0.000 description 2
- 241000018646 Pinus brutia Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 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
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 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
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000000344 soap 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)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a method for preparing light-color disproportionated rosin by using a phosphoric acid compound ceramsite decolorising agent. The method comprises the steps of: 1) transferring the rosin from a sedimentation tank to a dissolver for dissolving, and sending the dissolved grease liquid into a clarification tank; 2) introducing protection gas, standing the dissolved grease liquid in the clarification tank static to automatically stratify the grease liquid and water, and sending the clarified grease liquid into a reactor; 3) in an inert gas environment, heating the reactor to 250-270 DEG C; 4) maintaining the protection gas environment, reducing the temperature to below 160 DEG C, and adding a palladium carbon ceramic catalyst and a phosphoric acid compound ceramsite decolorising agent; 5) maintaining the protection gas environment, and heating to 280-290 DEG C; and 6) reducing the temperature, and filtering the product in liquid state to remove the catalyst and decolorising agent mixed in the reaction product to obtain the light-color disproportionated rosin. The method for preparing light-color dispropriated rosin reduces the amount of catalyst in posttreatment, and reduces production cost, and the disproportionated rosin has higher acid value, lighter color and higher yield.
Description
Technical field
The invention belongs to Colophonium field of deep, particularly relate to a kind of with phosphoric acid composite haydite decolorising agent preparation light color discrimination
The method changing Colophonium.
Background technology
Colophonium is a kind of reproducible natural resin, is described as " lignicolous oil ", is that important forest chemical produces
One of product.Colophonium is widely used in coating, the vigorous agent of glue, ink, papermaking, soap, intermetallic composite coating, synthetic rubber, building materials, food,
The industry such as macromolecule, fine chemical product.The quality of Colophonium is mainly determined by its color, acid number, softening point, transparency etc., typically
In the case of, the Colophonium that color is the most shallow, quality is the best, and rank is the highest, applied widely, and price is the highest.
The method preparing pale rosin mainly has Physical and chemical method, and physical method includes adsorption decoloring method, crystallization extraction
Follow the example of.Adsorption decoloring method DeGrain, and Colophonium loss is big, adsorbent is the most disposable;Crystalline extraction method quantity of solvent is big.Change
Method includes concentrated sulphuric acid decoloring method and saponification method;Concentrated sulphuric acid decoloring method needs to be filtered to remove carbon slag, will use substantial amounts of hydrocarbon
Kind solvent;The decolorizing effect of saponification method is unsatisfactory.
The most so-called colourless Colophonium color is about No. two colors, and color is shallower, less stable, range of application
Less, it is particularly unsuitable for some adhesive and coating industry.
Summary of the invention
The goal of the invention of the present invention is that providing a kind of prepares pale disproportionated rosin with phosphoric acid composite haydite decolorising agent
Method.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
A kind of method preparing pale disproportionated rosin with phosphoric acid composite haydite decolorising agent, the method includes:
1) Colophonium is put into Sedimentation tank, with conveying worm, Colophonium is delivered to dissolvers and dissolve, during dissolving, add Oleum Terebinthinae and water,
Leading to into steam during dissolving, temperature controls at 90-95 DEG C；The fat liquid dissolved defecator in dissolvers removes thick impurity
Rear entrance defecator;
2) being passed through protection gas, the fat liquid of dissolving stands 6-8 hour in defecator, makes fat liquid and water self exfoliation, discharges lower floor
Water, upper strata fat liquid is standing fat liquid, and the standing fat liquid after clarification is sent to reactor directly as the raw material of dismutation reaction;
3) in the environment of protection gas, reactor is warmed up to 250-270 DEG C, and stirring is incubated 30-60 minute;
4) maintain protection compression ring border, temperature of reactor is down to less than 160 DEG C, be slowly added into palladium carbon ceramsite catalyst and phosphoric acid is multiple
Compound haydite decolorising agent, stirring, described phosphoric acid composite haydite decolorising agent is that phosphoric acid composite decolorizer is attached to porous pottery
Prepare in grain surface and micropore;
5) maintain protection compression ring border, be warmed up to 280 DEG C-290 DEG C, be incubated 120-240 minute;
6) reduce temperature, and be filtered to remove the catalyst being mixed with in product and decolorising agent when product is in liquid, i.e. make
Obtain pale disproportionated rosin.
The above-mentioned method preparing pale disproportionated rosin, wherein, the gross mass of described Oleum Terebinthinae and water is Colophonium quality
0.5～0.7 times；The Oleum Terebinthinae stated is 1:3～1:6 with the mass ratio of water.
The above-mentioned method preparing pale disproportionated rosin, wherein, the Oleum Terebinthinae being evaporated in described Colophonium course of dissolution
Reclaim by the condenser on dissolvers top with steam.
The above-mentioned method preparing pale disproportionated rosin, wherein, water and the terebinthine steam of the effusion of described defecator enter
Enter condenser to reclaim, the slag-water slurry of bottom, discharged by stable can；Moisture, fine impurities and a small amount of dark-coloured Colophonium are formed
Intermediate layer be sent into middle-layer resin liquid defecator, reclaim fat liquid therein.
The above-mentioned method preparing pale disproportionated rosin, wherein, the described palladium a diameter of 0.1-1mm of carbon ceramsite catalyst, institute
State the phosphoric acid composite a diameter of 0.1-1mm of haydite decolorising agent.
Currently preferred technical scheme is: the above-mentioned method preparing pale disproportionated rosin, and described phosphoric acid composite is made pottery
Grain decolorising agent is that phosphoric acid composite is dissolved in Ludox, dispersion, and porous ceramic grain puts Ludox dipping into 1-3 hour, 40-
Dry and prepare for 120 DEG C.
Further preferred technical scheme is: the above-mentioned method preparing pale disproportionated rosin, and described phosphoric acid composite takes off
Toner is to mix with phosphoric acid, carbamide or quaternary ammonium salt for raw material；Described phosphoric acid composite decolorizer is phosphoric acid and carbamide is
Raw material mixes, then phosphoric acid and urea quality are than for 3:1-6:1；Described phosphoric acid composite decolorizer is phosphoric acid and quaternary ammonium salt is
Raw material mixes, then phosphoric acid and quaternary ammonium salt mass ratio are 1:1-3:1.
Further preferred technical scheme is: the described method preparing disproportionated rosin, it is characterised in that: phosphoric acid is combined
Thing, Ludox, haydite mass ratio are 0.2～1.5:4～5:1.
The above-mentioned method preparing pale disproportionated rosin, wherein, described protection gas is noble gas or nitrogen.
The above-mentioned method preparing pale disproportionated rosin, wherein, in described palladium carbon, the weight percent content of palladium be 3%～
5%。
The above-mentioned method preparing pale disproportionated rosin, wherein, described step 3) in, mixing speed is 300～500 turns/
min。
The above-mentioned method preparing pale disproportionated rosin, wherein, described step 6) in, temperature is reduced to 200～250 DEG C.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows:
1) method preparing pale disproportionated rosin of the present invention, uses first Colophonium high-temperature process, makes Colophonium at high temperature occur
Dismutation reaction, after allowing part abietic acid change into dehydroabietic acid, then carries out subsequent treatment so that the consumption of catalyst in late phase reaction
Substantially reduce, be effectively reduced production cost；
2) method preparing disproportionated rosin of the present invention, dismutation reaction is carried out under protection gas, it is to avoid Colophonium is oxidized, simultaneously
Have employed phosphoric acid composite haydite decolorising agent, effectively disproportionated rosin can be decoloured, significantly provide the matter of disproportionated rosin
Amount, makes disproportionated rosin color reach, about a color, can preferably be applied in some adhesive and coating industry；
3) method preparing pale disproportionated rosin of the present invention, uses palladium carbon ceramsite catalyst and the decolouring of phosphoric acid composite haydite
Agent, specific surface area is big, makes catalytic efficiency higher；Haydite easily filters removal relatively greatly, thus improves the quality of product；
4) disproportionated rosin that the method preparing pale disproportionated rosin of the present invention prepares, acid number is higher, color is more shallow, and productivity is more
High；
5) method preparing pale disproportionated rosin of the present invention, with Colophonium directly as dismutation reaction raw material, eliminates by fat liquid
Making the process of Colophonium, thus simplify flow process, investment reduction also reduces cost, it is thus also avoided that heating and melting makes product face repeatedly
The problem that complexion changed is deep.
Accompanying drawing explanation
Fig. 1 is the present invention；Prepare the flow chart of the method for pale disproportionated rosin.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is further described.
Embodiment 1
1) 2 tons of Colophonium are put into Sedimentation tank, with conveying worm, Colophonium is delivered to dissolvers and dissolve, during dissolving, add 600kg pine
Fuel-economizing and 600kg water, lead to into steam during dissolving, temperature controls at 90 DEG C, and the Oleum Terebinthinae being evaporated in course of dissolution and water steam
Gas is reclaimed by the condenser on dissolvers top；The fat liquid dissolved enters after the defecator in dissolvers removes thick impurity
Defecator;
2) being passed through nitrogen, the fat liquid of dissolving stands 6 hours in defecator, makes fat liquid and water self exfoliation, discharges lower layer of water, on
Layer fat liquid is standing fat liquid, and the standing fat liquid after clarification is sent to reactor directly as the raw material of dismutation reaction;Defecator escapes
The water gone out and terebinthine steam enter condenser and reclaim, and the slag-water slurry of bottom is discharged by stable can.Moisture, tiny
The intermediate layer that impurity and a small amount of dark-coloured Colophonium are formed is sent into middle-layer resin liquid defecator, reclaims fat liquid therein；
3) in the environment of nitrogen, reactor is warmed up to 250 DEG C, and mixing speed is 300 turns/min, is incubated 30 minutes;
4) maintain nitrogen environment, cool the temperature to 160 DEG C, be slowly added into palladium carbon ceramsite catalyst and the decolouring of phosphoric acid composite haydite
Agent, stirring;Phosphoric acid composite decolorizer is to mix with phosphoric acid quaternary ammonium salt for raw material, and phosphoric acid and quaternary ammonium salt mass ratio are 1:1；
5) maintain nitrogen environment, be warmed up to 280 DEG C, be incubated 120 minutes；
6) when temperature is reduced to 200 DEG C, product is put in filter, and be filtered to remove reaction when product is in liquid
The catalyst being mixed with in product and decolorising agent, i.e. prepare pale disproportionated rosin.
Embodiment 2
1) 4 tons of Colophonium are put into Sedimentation tank, with conveying worm, Colophonium is delivered to dissolvers and dissolve, during dissolving, add 1200kg pine
Fuel-economizing and 1200kg water, lead to into opening steam during dissolving, temperature controls at about 95 DEG C, the Lignum Pini Nodi being evaporated in course of dissolution
Oil and steam are reclaimed by the condenser on dissolvers top；The fat liquid defecator in dissolvers dissolved removes thick miscellaneous
Defecator is entered after matter；
2) being passed through nitrogen, the fat liquid of dissolving stands 8 hours in defecator, makes fat liquid and water self exfoliation, discharges lower layer of water, on
Layer fat liquid is standing fat liquid, and the standing fat liquid after clarification is sent to reactor directly as the raw material of dismutation reaction;Defecator escapes
The water gone out and terebinthine steam enter condenser and reclaim, and the slag-water slurry of bottom is discharged by stable can；Moisture, tiny
The intermediate layer that impurity and a small amount of dark-coloured Colophonium are formed is sent into middle-layer resin liquid defecator, reclaims fat liquid therein；
3) in the environment of nitrogen, reactor is warmed up to 270 DEG C, and mixing speed is 500 turns/min, is incubated 60 minutes;
4) maintain nitrogen environment, cool the temperature to 150 DEG C, be slowly added into palladium carbon ceramsite catalyst and the decolouring of phosphoric acid composite haydite
Agent, stirring;Phosphoric acid composite decolorizer is to mix with phosphoric acid and carbamide for raw material, and phosphoric acid and urea quality are than for 3:1；
5) maintain nitrogen environment, be warmed up to 290 DEG C, be incubated 240 minutes；
6) when temperature is reduced to 250 DEG C, product is put in filter, and be filtered to remove reaction when product is in liquid
The catalyst being mixed with in product and decolorising agent, i.e. prepare pale disproportionated rosin.
Table 1: disproportionated rosin quality and national standard comparison obtained by this law are as follows:
| Project | National standard (one-level) | Embodiment 1 | Embodiment 2 |
| Gardner's colorimetric≤ | 4 | 4 | 4 |
| Outward appearance | Transparent | Transparent | Transparent |
| Abietic acid content (%) ,≤ | 0.1 | 0.1 | 0.1 |
| Dehydrogenation abietic acid content (%) >= | 52 | 55 | 52 |
| Softening point (ring and ball method)/DEG C, >= | 76 | 77 | 76 |
| Acid value a/(mg/g), >= | 160 | 165 | 165 |
| Unsaponifiable matter content b/ (%) ,≤ | 10 | 10 | 10 |
| Alcohol-insoluble substance/(%) ,≤ | 0.030 | 0.030 | 0.030 |
| Ash/(%) ,≤ | 0.020 | 0.020 | 0.020 |
Add phosphoric acid composite haydite decolorising agent and palladium carbon ceramsite catalyst by above-mentioned course of reaction, make pale disproportionated rosin exist
Reactor is carried out decolour simultaneously and disproportionation processes, make the color and luster of pale rosin reach No. one to before the most colourless, and stability obtains
To improving significantly, some adhesive higher to color and luster requirement and coating industry can be directly applied to.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, on the premise of without departing from the technology of the present invention principle, it is also possible to make some improvement and replacement, these improve and replace
Also should be regarded as protection scope of the present invention.
Claims (10)
1. the method preparing pale disproportionated rosin with phosphoric acid composite haydite decolorising agent, it is characterised in that the method includes:
1) Colophonium is put into Sedimentation tank, with conveying worm, Colophonium is delivered to dissolvers and dissolve, during dissolving, add Oleum Terebinthinae and water,
Leading to into steam during dissolving, temperature controls at 90-95 DEG C；The fat liquid dissolved defecator in dissolver removes thick impurity
Rear entrance defecator;
2) being passed through protection gas, the fat liquid of dissolving stands 6-8 hour in defecator, makes fat liquid and water self exfoliation, after clarification
Clean fat liquid processed is sent to reactor directly as the raw material of dismutation reaction;
3) in the environment of protection gas, reactor is warmed up to 250-270 DEG C, is incubated 30-60 minute;
4) maintain protection compression ring border, cool the temperature to less than 160 DEG C, be slowly added into palladium carbon ceramsite catalyst and phosphoric acid composite pottery
Grain decolorising agent, prepares in palladium-carbon catalyst is attached to porous ceramic grain surface and micropore by described palladium carbon ceramsite catalyst;
5) maintain protection compression ring border, be warmed up to 280 DEG C-290 DEG C, be incubated 120-240 minute;
6) reduce temperature, and be filtered to remove the catalyst being mixed with in product and decolorising agent when product is in liquid, i.e. make
Obtain pale disproportionated rosin.
The method preparing pale disproportionated rosin the most as claimed in claim 1, it is characterised in that described Oleum Terebinthinae and total matter of water
Amount is 0.5～0.7 times of Colophonium quality;Described Oleum Terebinthinae is 1:1～1:3 with the mass ratio of water.
The method preparing pale disproportionated rosin the most as claimed in claim 1, it is characterised in that steam in described Colophonium course of dissolution
The Oleum Terebinthinae and the steam that issue are reclaimed by the condenser of dissolver；Water and the terebinthine steam of the effusion of described defecator enter
Entering condenser to reclaim, slag-water slurry is discharged.
The method preparing pale disproportionated rosin the most according to claim 1, it is characterised in that: described palladium carbon ceramsite catalyst
A diameter of 0.1-1mm, the described phosphoric acid composite a diameter of 0.1-1mm of haydite decolorising agent.
The method preparing pale disproportionated rosin the most according to claim 1, it is characterised in that described phosphoric acid composite decolours
Agent is to mix with phosphoric acid, carbamide or quaternary ammonium salt for raw material；Described phosphoric acid composite decolorizer is phosphoric acid and carbamide is former
Material mixes, then phosphoric acid and urea quality are than for 3:1-6:1；Described phosphoric acid composite decolorizer is phosphoric acid and quaternary ammonium salt is former
Material mixes, then phosphoric acid and quaternary ammonium salt mass ratio are 1:1-3:1.
The method preparing pale disproportionated rosin the most as claimed in claim 1, wherein, described phosphoric acid composite haydite decolorising agent is
Phosphoric acid composite is dissolved in Ludox, dispersion, and porous ceramic grain puts Ludox dipping into 1-3 hour, 40-120 DEG C dry and
Prepare.
The method preparing pale disproportionated rosin the most according to claim 1, it is characterised in that: described protection gas is indifferent gas
Body or nitrogen.
The method preparing pale disproportionated rosin the most according to claim 1, it is characterised in that: in described palladium carbon, the weight of palladium
Amount degree is 3%～5%.
The method preparing pale disproportionated rosin the most according to claim 1, it is characterised in that: step 3) in, mixing speed
It is 300～500 turns/min.
The method preparing pale disproportionated rosin the most according to claim 1, it is characterised in that: described step 6) in, temperature
Degree is reduced to 200～250 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610385125.XA CN106010273A (en) | 2016-06-03 | 2016-06-03 | Method for preparing light-color disproportionated rosin by using phosphoric acid compound ceramsite decolorising agent |
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|---|---|---|---|
| CN201610385125.XA CN106010273A (en) | 2016-06-03 | 2016-06-03 | Method for preparing light-color disproportionated rosin by using phosphoric acid compound ceramsite decolorising agent |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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