CN1245192A - Process for preparing hydrogenated rosin - Google Patents
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- CN1245192A CN1245192A CN 98115885 CN98115885A CN1245192A CN 1245192 A CN1245192 A CN 1245192A CN 98115885 CN98115885 CN 98115885 CN 98115885 A CN98115885 A CN 98115885A CN 1245192 A CN1245192 A CN 1245192A
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Abstract
A process for preparing hydrogenated rosin includes such steps as dissolving rosin or pine oleoresin in solvent, continuously hydrogenating on industrilized fixed bed under the existence of catalyst, and then separation. Its advantages include short reaction time, high output rate, long service life of catalyst and continuous production. The product features stable and high quality, light colour, very low content of abietic acid, high content of tetrahydroresin acid, and high deoxidizing nature and stability.
Description
The present invention relates to a kind of manufacture method of staybelite, particularly a kind of highly hydrogenated rosin or local hydriding's rosiny manufacture method.Rosin is the important source material of papermaking, paint, bonding, printing ink and other industrial sector.But the rosin softening temperature is lower, and easily crystallization has two two keys in the molecular structure, and particularly the abietic type acid has conjugated double bond structures, and is easily oxidized, and rosin oxidation-resistance and thermostability descend, and its application is restricted.In order to improve rosiny stability, often, change its double bond structure, make its double key number order reduce or eliminate double bond structure by reactions such as disproportionation, polymerization, hydrogenations, thereby improve its scale resistance, hydrogenation is to change the most effective a kind of method of resinous acid double bond structure in the rosin.The present staybelite narrated of suitability for industrialized production and relevant patent documentation, dihydro body resinous acid is at 60-80% in its chemical constitution, tetrahydrochysene body resinous acid is at the staybelite of 10-30%, and belonging to the dihydroabietic acid is main local hydriding's rosin (Partially Hydrogenated Rosin); Dihydro body resinous acid content is at 20-50% in its chemical constitution, and tetrahydrochysene body resinous acid content is at the staybelite of 40-80%, and belonging to tetrahydroabietic acid is main highly hydrogenated rosin.CN1093728A patent application and the U.S. one tame factory are raw material with rosin, adopting the fusion legal system is that the staybelite of principal constituent is that the method for carrying out hydrogenation after the molten rosin is fused in the rosin heating with tetrahydrochysene body resinous acid, except hydrogenation catalyst is had the particular requirement, carry out the reaction of secondary high-temperature and high-pressure hydrogenation, hydrogenation temperature reaches 240-280 ℃, hydrogenation pressure and reaches 32MPa, hydrogenation conditions is required high.In order to improve color grade, remove in the rosin coloring matter and to the deleterious impurity of catalyzer, keep catalyst activity, prolong the work-ing life of catalyzer, also will carry out molecular distillation, distillation temperature is 200-300 ℃, distillation pressure 0.13-1.3KPa (absolute pressure), the rosin rate of recovery of this production technique is lower, and energy consumption is big, high vacuum system equipment requirements height, Production Flow Chart is long, the production cost height.Patent application CN1097448A adopts crystallisation by cooling decolouring, solvent cut shortening, filtration, and low-temperature distillation obtains dihydro or tetrahydrochysene gum resin.This thermopnore owned by France is the hydrogenation flow process intermittently, raw material is a rosin, with making clean fat liquid after the turps dissolving, material liquid is cooled to 28-32 ℃ from 90-95 ℃ and kept 8-12 hour again, isolated crystallization is made catalyzer at the palladium charcoal that contains palladium 0.05% after with dissolution with solvents, is to carry out hydrogenation under charging capacity 0.2% condition at catalyst levels, when hydrogen pressure at 3-6MPa, temperature is produced dihydro rosin in the time of 130-170 ℃; Under same catalyst, when hydrogen pressure during at 160-200 ℃, is produced tetrahydrochysene rosin in 6-10MPa, temperature.Though this method adopts the decoloring method of crystallisation by cooling can improve the color of raw material, improves the look level of product, crystallisation by cooling is chronic, and usually more than 48 hours, and the crystalline yield only has 60-67%, and the Crystallization Separation difficulty is difficult to reach industrialized level.Under the hydrogenation conditions of this method, stablizing the tetrahydroabietic acid content that keeps in the product, to reach requirement be difficult.The batch production flow process is carried out hydrogenation to rosin liquid at intermittence in the hydrogenation reaction kettle; carry out several times nitrogen, hydrogen exchange behind raw material and the catalyst by proportion input reactor; under agitator stirs, boost, heat up and react then; adopt constant-voltage method or the heating method of boosting to keep the hydrogenation pressure of resinous acid; through 3-8 hour reaction, after the sampling detection is qualified, could shut down discharging; recovery part is used nitrogen replacement after reacting remaining hydrogen, removes by filter catalyzer and obtains product.After reusing 3-5 time, isolated catalyzer needs to change recycling separately.In order to maintain a certain amount of solution-air contact and mixing effect, the hydrogen in the reactor has accounted for the volume of 20-40%, and the useful volume of reactor is descended, and facility investment increases; Because intermittently hydroprocessing has comprised input and output material, gas displacement, boost, intensification, hydrogenation reaction, filtration etc., institute is so that prolong hydrogenation total time, under same industrial scale, require the volume of hydrogenation still big, investment is many, and floor space is big, and schedule of operation is numerous and diverse, operative employee's quantity is big, and labor strength is big.In addition, every pot of input and output material all will carry out gas displacement, this hydrogen partial, nitrogen are wasted in a large number, the catalyzer of interrupter method is short work-ing life, reclaiming also makes the catalyzer consumption big often, and compressor power consumption is also bigger in addition, production is difficult to carry out automatization control, the less stable of quality product.
The objective of the invention is to invent that a kind of technology is simple, reaction times weak point, catalyzer long service life, can continuous production, the manufacture method of constant product quality, staybelite that production cost is low.
Staybelite manufacture method of the present invention is characterized in that it makes raw material with dissolution with solvents rosin or rosin, under the catalyzer condition, through industrialization fixed bed continuous hydrogenation, and then separates and obtains staybelite, may further comprise the steps:
(1) rosin or rosin are made stock liquid with dissolution with solvents, preparation condition is:
Melting temperature (Tm): 80-150 ℃
The rosin content of feed liquid: 30-80%
The content of impurities of feed liquid: less than 0.1%
(2) feed liquid is carried out hydrogenation reaction in following condition, obtains hydrogenated mixture:
Hydrogenation mode: gas-solid-liquid three-phase fixed bed continous way shortening
Hydrogenation temperature: 170-260 ℃
Hydrogenation reaction pressure: 10-20MPa
Hydrogenation time: 0.5-2 hour
Catalyzer: palladium-charcoal, reduced nickel, rhodium.
(3) hydrogenated mixture that step (2) is obtained separates, and makes highly hydrogenated rosin or local hydriding's rosin; Isolated solvent cycle is used, and rectifying is got cis-pinane, alkane is made byproduct.
The raw material of the inventive method is that Pinus massoniana Lamb rosin, Pinus massoniana Lamb and slash pine mix rosin or their rosin product.Solvent can select for use pinane, kautschin, turps, hydroterpin wherein one or more.
The hydrogenation of the inventive method is to carry out continuously in fixed-bed reactor, belongs to gas-solid-liquid phase reaction, and input and output material is operate continuously.Miscellaneous equipment has dissolution kettle, continuous measurement charger, preheater, vapor-liquid separation groove, distiller, rectifying tower, electrolysis hydrogen production device, hydrogen gas compressor and circulator, is conventional equipment.
Rosin (or rosin) is made the stock liquid that concentration is 30-80% with the dissolving under 90-150 ℃ of pinane, turps, kautschin, in the continuous measurement fresh feed pump is evenly delivered to preheater and mixing tank, feed liquid with enter the fixed bed catalyst hydrogenator after hydrogen mixes, hydrogenation under the following conditions:
100-200 ℃ of feed liquid preheating temperature
60-150 ℃ of hydrogen preheating temperature
Hydrogen purity 〉=99%
170-260 ℃ of hydrogenation temperature
Hydrogenation reaction pressure 10-20MPa
Reaction times 0.5-2 hour
Vapour-liquid ratio is greater than 2000
Palladium catalyst-charcoal, reduced nickel, rhodium, the every batch of 300-400 kilogram that feeds intake
Space velocity 0.4-0.8
The hydrogenation mode is gas-solid-and liquid three-phase fixed bed continous way shortening adds hydrogen mixture after solution-air is separated, and hydrogen is sent reactive system back to recycle compressor, and the hydrogenation mixed solution obtains highly hydrogenated rosin behind vacuum distillation recovered solvent in distiller.Isolated solvent cycle is used, and separablely goes out cis-pinane, alkane is made byproduct with rectificating method.The condition of separated from solvent is: distillation temperature 150-180 ℃, and vacuum tightness 0.03-0.08MPa, 150-250 ℃ of working steam temperature, working steam pressure 0.05-0.155MPa, 250-320 ℃ of thermal oil temperature.Resinous acid generates dihydro body resinous acid and tetrahydrochysene body resinous acid through hydrogenation reaction, its tetrahydrochysene body resinous acid content of the highly hydrogenated rosin that makes is at 40-75%, abietic acid content is at 0-1%, dehydrogenation abietic acid 4-6%, acid number 162-168 (mg.KOH/g), 74-78 ℃ of softening temperature (ring and ball method), alcohol-insoluble substance content is at 0.01-0.03%, color is at 2-4 (Gardner look number), and product oxidation-resistance and thermostability are fabulous.
Adjust type of solvent and fat liquid concentration, change hydrogenation conditions, preparation local hydriding rosin under following condition.
90-120 ℃ of material melting temperature (Tm)
The rosin content 50-80% of stock liquid
The trans pinane of solvent, kautschin, turps, hydroterpin
Palladium catalyst-charcoal, reduced nickel, rhodium, the every batch of 300-400 kilogram that feeds intake
Space velocity 0.4-0.8
100-180 ℃ of stock liquid preheating temperature
100-200 ℃ of hydrogen preheating temperature
170-230 ℃ of hydrogenation temperature
Hydrogenation reaction pressure 7-15MPa
Reaction times 0.5-1.5 hour
Vapour-liquid ratio is greater than 2000
The distillation temperature 160-180 of separated from solvent ℃
Distillatory vacuum tightness 0.03-0.08MPa
250-320 ℃ of working steam temperature
The content of its tetrahydrochysene body resinous acid of local hydriding's rosin of preparation is at 25-45%, dihydro body resinous acid content is at 55-70%, abietic acid content 0.5-1.5%, dehydroabietic acid content 5-8%, color 4-6 (Gardner), 72-74 ℃ of softening temperature (ring and ball method), acid number 162-164 (mg.KOH/g), the product antioxidant property is good.Separated from solvent adopts steam distillation, underpressure distillation, rectifying; The refining packing tower that adopts of pinane.
The present invention is a raw material with dissolution with solvents rosin or rosin solution, under the catalyzer condition, through fixed bed continous way hydrogenation, adds hydrogen mixture and obtains highly hydrogenated rosin or local hydriding's rosin again after separating.The abietic type acid accounts for 75-85% in the Pinus massoniana Lamb gum resin, pimaric type acid accounts for 10-25%, also contain a spot of lipid acid and neutral substance, more change catalyzer and hydroconversion condition, hydrogenated resin acid content considerable change in the product, tetrahydrochysene body resinous acid is principal constituent with tetrahydroabietic acid and tetrahydropimaric acid.Its reaction formula is:
Tetrahydroabietic acid tetrahydropimaric acid dihydro body resinous acid is compositions such as dihydroabietic acid, dihydropimaric acid, dihydroisopimaric acid.Its reaction formula is:
Dihydroabietic acid's dihydropimaric acid dihydroisopimaric acid tetrahydrochysene body resinous acid content height, the double bond containing number of resinous acid institute is few in the rosin, rosiny oxidation-resistance and thermostability raising, of light color.
Producer of the present invention continous way solvent method owned by France, material is sent into system with the high-pressure pump continuously and smoothly, feed liquid is through mixing with the hydrogen of being sent into by hydrogen gas compressor and circulator in mixing tank after the preheating and together entering reactor, under certain pressure, temperature, carry out hydrogenation, after the hydrogenation mixture separation goes out hydrogen, solvent, make highly hydrogenated pine or local hydriding's incense products, hydrogen recycle is used.Solvent method can reduce the viscosity of reactant, the resistance of the infiltration of hydrogen molecule in reaction medium, diffusion is little, gas (hydrogen) Gu-(catalyzer)-liquid (resinous acid solution) three contacts well, helps the hydrogenation of resinous acid molecule, short, hydrogenation temperature of reaction times and pressure are lower, hydrogenation conditions is gentle, the catalyzer long service life, prepared highly hydrogenated rosin is of light color, tetrahydrochysene body resinous acid content height, abietic acid content is extremely low, the oxidation-resistance of product and Heat stability is good.Fixed bed continous way shortening, reaction mass charging equilibrium, stable, the gas pushing quantity of its hydrogen gas compressor is only for replenishing required hydrogen of rosin hydrogenation and hydrogen losses such as system leak, dissolving, gas pushing quantity can be saved facility investment and process cost much smaller than adopting the required hydrogen gas compressor gas pushing quantity of discontinuous method; Adopt the serialization flow process, facility compact, volume is little, the total floor space of system is little, realizes that easily automatization, labor strength are low.
Embodiment 1
Clarified resin liquid (temperature 85-95 ℃ contains rosin amount 58-65%) during rosin factory produced is with 0.4-0.7m
3The inlet amount of/h is injected hydrogenation system continuously, fat liquid be preheated to 100-200 ℃ with enter in the reactor after hydrogen mixes, catalyzer is the fixed bed pattern, space velocity is 0.4-0.8, controls each temperature of reactor at 180-250 ℃, and each section reactor temperature difference is less than 10 ℃, be and increase progressively layout, hydrogenation reaction pressure is controlled at 10-16MPa, and vapour-liquid ratio is greater than 2000, and the reaction times was at 1-2 hour.Hydrogen purity is more than 99%, and separated hydrogen is used by hydrogen recycle machine delivery cycle, when contained amount of carbon dioxide in the hydrogen is big, opens washing water and removes carbonic acid gas.Rosin mixed solution behind the hydrogenation is isolated hydroterpin through steam distillation in still pot, distillation temperature 160-180 ℃, vacuum tightness/0.03-0.08MPa, 250-360 ℃ of working steam temperature, working steam pressure 0.05-0.15MPa, hydroterpin can be made solvent cycle and use, and also rectifiable production pinane or cis-pinane are sold.The tower top temperature 80-115 of pinane rectifying ℃, column bottom temperature 120-165 ℃, vacuum tightness 0.05-0.092MPa, reflux ratio 1.5-3.5.
Making 72-74 ℃ of its softening temperature of highly hydrogenated rosin, acid value 162-164mgKOH/g, outward appearance is transparent solid, color 3-6 (Gardner), abietic acid content 0-2%, dehydroabietic acid content 4-8%, impurity 0.02-0.025%, alcohol-insoluble substance 0.013-0.018%, unsaponifiables 5.2-6.5%, tetrahydrochysene body resinous acid content 40-60%, dihydro body resinous acid 31～38%, the product antioxidant property is good.Embodiment 2
The molten state heat perfume that rosin factory tallow rendering workshop distillation plant is emitted is made rosin solution with pinane, kautschin dissolving in dissolver, the requirement raw material is one-level, secondary rosin, and the resinous acid content of solution is at 40-80%, melting temperature (Tm) 90-150 ℃, foreign matter content is less than 0.1%, with 0.2-0.8m
3The inlet amount of/h is continuous, the balanced hydrogenation system that injects, material enters in the reactor in mixing tank with after hydrogen mixes through being preheated to 100-200 ℃, catalyst in reactor is a fixed bed catalyst, every batch of catalyzer charging capacity is the 300-400 kilogram, space velocity is 0.4-0.8, control each reactor hydrogenation temperature at 180-260 ℃, each reactor temperature difference is less than 10 ℃, temperature is presented control, hydrogenation reaction pressure is controlled at 12-20MPa, vapour-liquid ratio is greater than 2500, and in 1.5 hours reaction times, every batch of catalyzer work-ing life was at 3000 hours, hydrogen purity is more than 99%, separated hydrogen is used by the circulator delivery cycle, and replenishes the hydrogen of hydrogenation reaction consumes with the hydrogen pressure machine, keeps the hydrogen pressure of hydrogenation system.Rosin mixed solution underpressure distillation in still pot behind the hydrogenation is reclaimed solvent, and is recycled, and distillation temperature is at 150-180 ℃, vacuum tightness 0.03-0.08MPa, and rectifying is got cis-pinane, alkane is made byproduct.
Making 74-76 ℃ of its softening temperature of highly hydrogenated rosin, acid value 164-166mg.KOH/g, outward appearance and be transparent solid, color 2-4 (Gardner), impurity 0.02-0.025%, alcohol-insoluble substance 0.013-0.018%, unsaponifiables 5-6%, tetrahydrochysene body resinous acid content 50-75%, dihydro body resinous acid 20～30%, dehydroabietic acid 2-5%, abietic acid content is zero, and product oxidation-resistance and thermostability are fabulous.Embodiment 3
Rosin is made the stock liquid that contains rosin 50-80% with the fusion under 90-120 ℃ of hydroterpin, kautschin, and feed liquid is with 0.6-0.9m
3The inlet amount of/h is injected hydrogenation system continuously, fat liquid be preheated to 100-180 ℃ with enter in the reactor after hydrogen mixes, catalyzer is the fixed bed pattern, and every batch of catalyzer charging capacity is at the 300-350 kilogram, and space velocity is 0.4-0.8, control each temperature of reactor at 170-230 ℃, each section reactor temperature difference is less than 10 ℃, is to increase progressively layout, and hydrogenation reaction pressure is controlled at 7-15MPa, vapour-liquid ratio is greater than 2000, and the reaction times was at 0.5-1.5 hour.Hydrogen purity is more than 99%, and separated hydrogen is used by hydrogen recycle machine delivery cycle, when contained amount of carbon dioxide in the hydrogen is big, opens washing water and removes carbonic acid gas.Rosin mixed solution behind the hydrogenation is isolated hydroterpin through steam distillation in still pot, and distillation temperature 160-180 ℃, vacuum tightness 0.03-0.08MPa, 250-320 ℃ of working steam temperature, working steam pressure 0.05-0.15MPa, hydroterpin make solvent cycle and use.Making 72-74 ℃ of local hydriding's its softening temperature of rosin product, acid value 162-164mgKOH/g, outward appearance is transparent solid, color 4-6 (Gardner), impurity 0.02-0.025%, alcohol-insoluble substance 0.01-0.02%, unsaponifiables 5-6.5%, tetrahydrochysene body resinous acid content 25-45%, dihydro body resinous acid 55～70%, dehydroabietic acid content 5-8%, abietic acid content 1.5%, the product antioxidant property is good.
Highly hydrogenated rosin and the local staybelite produced by manufacture method of the present invention can be used for aspects such as printing-ink, hotmelt, caking agent, foodstuff additive, electronics soldering flux, senior paper size.
Claims (7)
1, a kind of manufacture method of staybelite is characterized in that it makes raw material with dissolution with solvents rosin or rosin, under the catalyzer condition, through industrialization fixed bed continuous hydrogenation, and then separates and obtains staybelite, may further comprise the steps:
(1) rosin or rosin are made stock liquid with the solvent fusion, preparation condition is:
Melting temperature (Tm): 80-150 ℃
The rosin content of feed liquid: 30-80%
The content of impurities of feed liquid: less than 0.1%
(2) feed liquid is carried out hydrogenation reaction in following condition, obtains hydrogenated mixture:
Hydrogenation mode: gas-solid-liquid three-phase fixed bed continous way shortening
Hydrogenation temperature: 170-260 ℃
Hydrogenation reaction pressure: 10-20MPa
Hydrogenation time: 0.5-2 hour
Catalyzer: palladium-charcoal, reduced nickel, rhodium.
(3) hydrogenated mixture that step (2) is obtained separates, and makes highly hydrogenated rosin or local hydriding's rosin; Isolated solvent cycle is used, and rectifying is got cis-pinane, alkane is made byproduct.
2, method according to claim 1 is characterized in that described raw material is that Pinus massoniana Lamb rosin, Pinus massoniana Lamb and slash pine mix rosin or their rosin product; Solvent select for use pinane, kautschin, turps, hydroterpin wherein one or more.
3, method according to claim 1 and 2 is characterized in that hydrogenation is to carry out continuously in fixed-bed reactor.
4, method according to claim 1 and 2 is characterized in that producing the main working condition of highly hydrogenated rosiny and is:
(1) feed liquid is carried out hydrogenation reaction under the following conditions:
90-150 ℃ of feed liquid melting temperature (Tm)
100-200 ℃ of feed liquid preheating temperature
The rosin content 30-80% of feed liquid
60-150 ℃ of hydrogen preheating temperature
180-260 ℃ of hydrogenation temperature
Hydrogenation reaction pressure 10-20MPa
Reaction times 0.5-2 hour
Space velocity 0.4-0.8
(2) the hydrogenation catalyst system therefor is palladium-charcoal, reduced nickel, rhodium, and carrier is wood activated charcoal or coal mass active carbon, and gac is powdery carbon, indefinite form particle charcoal or typing particle charcoal, the every batch of 300-400 kilogram that feeds intake.
(3) hydrogenation is a fixed bed continous way shortening, hydrogen purity require for hydrogen content greater than 99%, oxygen content is less than 0.5%, vapour-liquid ratio is greater than 2000.
(4) separated from solvent comprises steam distillation, rectifying or underpressure distillation.
(5) the heating thermal source adopts electrically heated, superheated vapour heating or heat-conducting oil heating.
5, method according to claim 8 is characterized in that producing the main working condition of highly hydrogenated rosiny and is:
(1) feed liquid is carried out hydrogenation reaction under the following conditions:
90-150 ℃ of feed liquid melting temperature (Tm)
100-200 ℃ of feed liquid preheating temperature
The rosin content 30-80% of feed liquid
60-150 ℃ of hydrogen preheating temperature
180-260 ℃ of hydrogenation temperature
Hydrogenation reaction pressure 10-20MPa
Reaction times 0.5-2 hour
Space velocity 0.4-0.8
(2) the hydrogenation catalyst system therefor is palladium-charcoal, reduced nickel, rhodium, and carrier is wood activated charcoal and coal mass active carbon, and gac is powdery carbon, indefinite form particle charcoal and typing particle charcoal, the every batch of 300-400 kilogram that feeds intake.
(3) hydrogenation is a fixed bed continous way shortening, hydrogen purity require for hydrogen content greater than 99%, oxygen content is less than 0.5%, vapour-liquid ratio is greater than 2000.
(4) separated from solvent comprises steam distillation, rectifying or underpressure distillation.
(5) the heating thermal source adopts electrically heated, superheated vapour heating or heat-conducting oil heating.
6, method according to claim 1 and 2 is characterized in that changing hydrogenation conditions, is applicable to local hydriding's rosiny production, and its underlying condition is as follows:
(1) rosin solution (or rosin solution) is carried out hydrogenation reaction under the following conditions:
90-150 ℃ of feed liquid melting temperature (Tm)
The rosin content 50-80% of feed liquid
Raw material preheating temperature 100-180 ℃
100-200 ℃ of hydrogen preheating temperature
170-230 ℃ of hydrogenation temperature
Hydrogenation reaction pressure 7-15MPa
Reaction times 0.5-1.5 hour
Space velocity 0.4-0.8
(2) the hydrogenation catalyst system therefor is palladium-charcoal, reduced nickel, rhodium, and carrier is wood activated charcoal and coal mass active carbon, and gac is powdery carbon, indefinite form particle charcoal or typing particle charcoal, the every batch of 300-400 kilogram that feeds intake.
(3) hydrogenation adopts fixed bed continous way shortening, and vapour-liquid ratio is greater than 2000, and the content of purity requirement hydrogen is greater than 99%, and oxygen content is less than 0.5%.
(4) separated from solvent comprises underpressure distillation, rectifying, steam distillation.
7, method according to claim 3 is characterized in that changing hydrogenation conditions, is applicable to local hydriding's rosiny production, and its underlying condition is as follows:
(1) rosin solution (or rosin solution) is carried out hydrogenation reaction under the following conditions:
90-150 ℃ of feed liquid melting temperature (Tm)
The rosin content 50-80% of feed liquid
Raw material preheating temperature 100-180 ℃
100-200 ℃ of hydrogen preheating temperature
170-230 ℃ of hydrogenation temperature
Hydrogenation reaction pressure 7-15MPa
Reaction times 0.5-1.5 hour
Space velocity 0.4-0.8
(2) the hydrogenation catalyst system therefor is palladium-charcoal, reduced nickel, rhodium, and carrier is wood activated charcoal or coal mass active carbon, and gac is powdery carbon, indefinite form particle charcoal or typing particle charcoal, the every batch of 300-400 kilogram that feeds intake.
(3) hydrogenation adopts fixed bed continous way shortening, and vapour-liquid ratio is greater than 2000, and the content of purity requirement hydrogen is greater than 99%, and oxygen content is less than 0.5%.
(4) separated from solvent comprises underpressure distillation, rectifying, steam distillation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98115885A CN1089353C (en) | 1998-08-13 | 1998-08-13 | Process for preparing hydrogenated rosin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98115885A CN1089353C (en) | 1998-08-13 | 1998-08-13 | Process for preparing hydrogenated rosin |
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| CN1245192A true CN1245192A (en) | 2000-02-23 |
| CN1089353C CN1089353C (en) | 2002-08-21 |
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| CN98115885A Expired - Lifetime CN1089353C (en) | 1998-08-13 | 1998-08-13 | Process for preparing hydrogenated rosin |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317347C (en) * | 2004-09-27 | 2007-05-23 | 广西大学 | Water-white hydrogenating rosin production |
| CN102002321A (en) * | 2010-12-06 | 2011-04-06 | 广西梧州日成林产化工股份有限公司 | Method for preparing colorless hydrogenated rosin ester resin |
| CN102070988A (en) * | 2011-01-20 | 2011-05-25 | 广西梧州日成林产化工股份有限公司 | Method for producing water-white hydrogenated rosin |
| CN103627324A (en) * | 2013-11-28 | 2014-03-12 | 广东科茂林产化工股份有限公司 | Preparation method of hydrogenated rosin without crystallization tendency |
| CN105752920A (en) * | 2016-05-20 | 2016-07-13 | 广西梧州日成林产化工股份有限公司 | Conveying method for hot rosin |
| CN109321269A (en) * | 2018-09-12 | 2019-02-12 | 广西大学 | The method that pine tree effluent cracked-hydrogenate simultaneously preparation bio oil and monoterpene alkane |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2790404B2 (en) * | 1993-03-26 | 1998-08-27 | 隆太郎 木下 | Method for producing hydrogenated rosin |
-
1998
- 1998-08-13 CN CN98115885A patent/CN1089353C/en not_active Expired - Lifetime
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317347C (en) * | 2004-09-27 | 2007-05-23 | 广西大学 | Water-white hydrogenating rosin production |
| CN102002321A (en) * | 2010-12-06 | 2011-04-06 | 广西梧州日成林产化工股份有限公司 | Method for preparing colorless hydrogenated rosin ester resin |
| CN102002321B (en) * | 2010-12-06 | 2013-05-08 | 广西梧州日成林产化工股份有限公司 | Method for preparing colorless hydrogenated rosin ester resin |
| CN102070988A (en) * | 2011-01-20 | 2011-05-25 | 广西梧州日成林产化工股份有限公司 | Method for producing water-white hydrogenated rosin |
| CN102070988B (en) * | 2011-01-20 | 2014-04-02 | 广西梧州日成林产化工股份有限公司 | Method for producing water-white hydrogenated rosin |
| CN103627324A (en) * | 2013-11-28 | 2014-03-12 | 广东科茂林产化工股份有限公司 | Preparation method of hydrogenated rosin without crystallization tendency |
| CN103627324B (en) * | 2013-11-28 | 2015-09-09 | 广东科茂林产化工股份有限公司 | A kind of preparation method of nodeless mesh trend staybelite |
| CN105752920A (en) * | 2016-05-20 | 2016-07-13 | 广西梧州日成林产化工股份有限公司 | Conveying method for hot rosin |
| CN105752920B (en) * | 2016-05-20 | 2019-02-15 | 广西梧州日成林产化工股份有限公司 | The delivery method of hot rosin |
| CN109321269A (en) * | 2018-09-12 | 2019-02-12 | 广西大学 | The method that pine tree effluent cracked-hydrogenate simultaneously preparation bio oil and monoterpene alkane |
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| CN1089353C (en) | 2002-08-21 |
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Address after: 543100 Guangxi Cangwu County town Guangxin Road No. 385 Patentee after: Wuzhou Sun Shine Forestry & Chemicals Co., Ltd. of Guangxi Address before: 543100 Guangxi Cangwu County town Guangxin Road No. 385 Patentee before: Guangxi Wuzhou Richeng Forest Products Chemical Co., Ltd. |
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