CN103214970A - Preparation method of pale rosin - Google Patents
Preparation method of pale rosin Download PDFInfo
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- CN103214970A CN103214970A CN2013101534938A CN201310153493A CN103214970A CN 103214970 A CN103214970 A CN 103214970A CN 2013101534938 A CN2013101534938 A CN 2013101534938A CN 201310153493 A CN201310153493 A CN 201310153493A CN 103214970 A CN103214970 A CN 103214970A
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Abstract
The invention provides a preparation method of pale rosin. The preparation method of the pale rosin comprises the following steps of: rinsing the rosin for 2-5 times with water, removing colloid, chlorophyll, trace sugar and protein in the rosin, feeding into a distillation tower, rising the temperature to 180-280 DEG C under the protection of inert gas so that the rosin is completely smelted, insulating for 1-4 hours, and cooling to 90-120 DEG C to obtain the pale rosin. The method is simple to operate, and low in energy consumption and cost, and chemical agents are not needed. The prepared rosin is pale in color, low in acid value, high in softening point, stable in quality, safe and pollution-free.
Description
Technical field
The present invention relates to a kind of rosiny manufacture method, relate generally to a kind of manufacture method of pale rosin.
Background technology
Rosin is the important foundation industrial chemicals of natural reproducible, has premium propertiess such as anticorrosion, moistureproof, insulation, bonding, emulsification, therefore is widely used in material, chemistry, each field of chemical industry.Rosin is the mixture of various kinds of resin acid and little fat acid and neutral substance, and wherein resinous acid is main component, accounts for more than 90% of its total amount.Resinous acid is that the molecule formula is the general name of the isomers of C19H29COOH, and they all have the luxuriant and rich with fragrance shelf structure of a triatomic ring, two two keys and a carboxyl, can be divided into conjugated double bond type resinous acid, unconjugated double bond type resinous acid and dehydrogenation, hydrogenated resin acid.Two key unstable chemcial properties, easily with atmosphere in the oxygen effect, oxygen absorbed can reach 10% of rosin weight, thereby makes the rosin color burn, the quality reduction.
Rosiny light colorization technological method mainly contains physics method and chemical method at present.The physics method comprises distillation method, adsorption decoloring method and crystallization extraction process.Distillation method is to make pale rosin by distillation method under vacuum state, and the too high rosin that causes easily of temperature decomposes in still-process, and the pale rosin oxygen uptake that makes is very big, returns look easily.Adsorption decoloring method is to come the rosin decolouring by the strong adsorption to coloring matter such as gac, activated earth and molecular sieve, but decolorizing effect is not obvious, and the rosin loss is bigger.Crystallization, extraction process are to utilize the difference of rosin acid and the solubleness of coloring matter in immiscible solvent to prepare pale rosin, but solvent load is bigger, and cost is higher.Chemical method generally adds light-colored agent such as phenols, phosphorous acid esters, the sulfur-bearing compounds makes rosin color aufhellung, but this method produces dehydroabietic acid by the rosiny disproportionation reaction, dihydroabietic acid or tetrahydroabietic acid and the colored oxide that reduces shoal the rosin color, but these light-colored agents can residue in the rosin, have serious toxic action for the custom catalysts in the rosin deep-processing process, as be used for food or daily necessities also can work the mischief to human body.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method that any chemicals is made pale rosin that need not to add.
Technical scheme provided by the invention is a kind of manufacture method of pale rosin; water rinse rosin 2～5 times of this method; remove colloid, chlorophyll, micro sugar and protein in the rosin; send in the distillation tower then; under protection of inert gas, progressively be warming up to 180～280 ℃ it is melted fully, be incubated 1～4 hour; be cooled to 90～120 ℃, be pale rosin.
Described water is the deionized water of distilled water or sterilization, and in the rinse cycle, each rinsing must renew water rinse with old water elimination.Rinse method can be to leave standstill intermittent type, also can be the continuously stirring formula.
Described rare gas element is nitrogen, helium or carbonic acid gas.
Rosin is in the process of heating, the turps gasification, collect turps after the condensation, continue to be warming up to 180～280 ℃, original coloring matter takes place to decompose or isomery in high-temperature process in the rosin, thereby the rosin color is shoaled, disproportionation takes place in the abietic type acid in the rosin in high-temperature process, the part dehydrogenation is converted into dehydroabietic acid, the hydrogen reduction that discharges the part coloring matter in the rosin, thereby make rosin color aufhellung.
Compared with prior art, the present invention has the following advantages:
1, the rinsed with deionized water rosin of employing distilled water or sterilization can be removed the impurity such as colloid, chlorophyll, micro sugar and protein in the rosin, has suppressed rosin brown stain in subsequent step.
2, charge into rare gas element in the distillation tower and obtain oxygen-free environment, make rosin and oxygen isolated, avoid the rosin brown stain.
3, any chemical additive of the different uses of the present invention does not have chemicals and remains in the rosin, is beneficial to rosiny following process and utilization, more safety and environmental protection.
4, present method is easy and simple to handle, less energy consumption, and expense is low, and rosin lighter color, the acid number that makes is low, softening temperature is high, steady quality.
Embodiment
The present invention is further elaborated for following specific embodiment, but not as a limitation of the invention.
Embodiment 1
1, rinsing: will send in the rosin pond after the fresh rosin fragmentation, add distilled water and leave standstill the intermittent type rinsing, the water surface should surpass fat face 20cm, changes a rinsing water in per 5 days, change 2 times continuously after, taking-up.
2, obtain vacuum environment: the rosin of rinsing is delivered in the distillation tower, closed intake valve, the boiling water pump vacuumizes, and removes the oxygen in the distillation tower as far as possible, closes vacuum valve behind the 5min after vacuumizing, and drives into and closes intake valve after air valve leads to nitrogen 2min.Repeat this step operation 3 times, close vacuum valve for the last time, logical nitrogen to distillation tower pressure inside is slightly larger than outside atmosphere, opens vacuum valve then, cuts out the pump.
3, open water of condensation, begin heating, when temperature rose to 180 ℃, rosin all melted, and was incubated 1 hour, was cooled to 90 ℃, was pale rosin, and look number is the National Standard Method secondary, and acid number is 167.9, and softening temperature (ring and ball method) is 81.0.
Embodiment 2
1, rinsing: will send in the rosin pond after the fresh rosin fragmentation, the deionized water that adds sterilization carries out the rinsing of continuously stirring formula, and the water surface should surpass fat face 30cm, changes a rinsing water in per 30 days, change 2～5 times continuously after, taking-up.
2, obtain vacuum environment: the rosin of rinsing is delivered in the distillation tower, closed intake valve, the boiling water pump vacuumizes, and removes the oxygen in the distillation tower as far as possible, closes vacuum valve after vacuumizing back 5min, closes intake valve after driving air valve helium injection gas 2min into.Repeat this step operation 3 times, close vacuum valve for the last time, helium injection gas to distillation tower pressure inside is slightly larger than outside atmosphere, opens vacuum valve then, cuts out the pump.
3, open water of condensation, begin heating, when temperature rose to 280 ℃, rosin all melted, and was incubated 4 hours, was cooled to 90～120 ℃, was pale rosin.Look number is the National Standard Method secondary, and acid number is 167.8, and softening temperature (ring and ball method) is 81.2.
Embodiment 3
1, rinsing: will send in the rosin pond after the fresh rosin fragmentation, add distilled water and leave standstill the intermittent type rinsing, the water surface should surpass fat face 25cm, changes a rinsing water in per 15 days, change 4 times continuously after, taking-up.
2, obtain vacuum environment: the rosin of rinsing is delivered in the distillation tower, closed intake valve, the boiling water pump vacuumizes, and removes the oxygen in the distillation tower as far as possible, closes vacuum valve behind the 5min after vacuumizing, and drives into and closes intake valve after air valve leads to carbonic acid gas 2min.Repeat this step operation 3 times, close vacuum valve for the last time, logical carbonic acid gas to distillation tower pressure inside is slightly larger than outside atmosphere, opens vacuum valve then, cuts out the pump.
3, open water of condensation, begin heating, when temperature rose to 220 ℃, rosin all melted, and was incubated 3 hours, was cooled to 100 ℃, was pale rosin.Look number is the National Standard Method one-level, and acid number is 167.1, and softening temperature (ring and ball method) is 81.6.
Embodiment 4
1, rinsing: will send in the rosin pond after the fresh rosin fragmentation, the deionized water that adds sterilization leaves standstill the intermittent type rinsing, and the water surface should surpass fat face 20cm, changes a rinsing water in per 30 days, change 2 times continuously after, taking-up.
2, obtain vacuum environment: the rosin of rinsing is delivered in the distillation tower, closed intake valve, the boiling water pump vacuumizes, and removes the oxygen in the distillation tower as far as possible, closes vacuum valve behind the 5min after vacuumizing, and drives into and closes intake valve after air valve leads to nitrogen 2min.Repeat this step operation 3 times, close vacuum valve for the last time, logical nitrogen to distillation tower pressure inside is slightly larger than outside atmosphere, opens vacuum valve then, cuts out the pump.
3, open water of condensation, begin heating, when temperature rose to 280 ℃, rosin all melted, and was incubated 1 hour, was cooled to 120 ℃, was pale rosin.Look number is the National Standard Method secondary, and acid number is 167.6, and softening temperature (ring and ball method) is 81.4.
Claims (4)
1. the manufacture method of a pale rosin; it is characterized in that: use water rinse rosin 2～5 times; remove colloid, chlorophyll, micro sugar and protein in the rosin; send in the distillation tower then; under protection of inert gas, progressively be warming up to 180～280 ℃ it is melted fully, be incubated 1～4 hour; be cooled to 90～120 ℃, be pale rosin.
2. the manufacture method of a kind of pale rosin according to claim 1, it is characterized in that: described water is the deionized water of distilled water or sterilization.
3. the manufacture method of a kind of pale rosin according to claim 1, it is characterized in that: described rare gas element is nitrogen, helium or carbonic acid gas.
4. the manufacture method of a kind of pale rosin according to claim 1, it is characterized in that: described rinsing is for leaving standstill intermittent type or the rinsing of continuously stirring formula.
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| CN2013101534938A CN103214970A (en) | 2013-04-28 | 2013-04-28 | Preparation method of pale rosin |
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| CN2013101534938A CN103214970A (en) | 2013-04-28 | 2013-04-28 | Preparation method of pale rosin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105086833A (en) * | 2015-09-29 | 2015-11-25 | 广西梧州日成林产化工股份有限公司 | Preparation method of polymerized rosin with high softening point |
| CN105860854A (en) * | 2016-05-13 | 2016-08-17 | 广西融水闽兴树脂有限公司 | Water-white rosin production line |
| CN106905855A (en) * | 2017-03-29 | 2017-06-30 | 南宁市青秀区嘉利林化有限公司 | The method that hydrogenated rosin is prepared from rosin |
| CN108789985A (en) * | 2018-04-28 | 2018-11-13 | 中国地质大学（北京） | Optimize the method and Chinese wax amber that Baltic amber prepares Chinese wax amber by heat |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337431A (en) * | 2001-09-03 | 2002-02-27 | 广西大学 | Ping gum processing potching and distilling method |
| CN1613940A (en) * | 2004-09-27 | 2005-05-11 | 广西大学 | Water-white hydrogenating rosin production |
| CN101362924A (en) * | 2008-10-08 | 2009-02-11 | 中国林业科学研究院林产化学工业研究所 | Method for decolorization preparation of pale rosin by rosin containing non-decoloring agent |
| CN101649160A (en) * | 2009-09-11 | 2010-02-17 | 广西民族大学 | Method for producing refined light-color rosin by using turpentine as raw material |
-
2013
- 2013-04-28 CN CN2013101534938A patent/CN103214970A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337431A (en) * | 2001-09-03 | 2002-02-27 | 广西大学 | Ping gum processing potching and distilling method |
| CN1613940A (en) * | 2004-09-27 | 2005-05-11 | 广西大学 | Water-white hydrogenating rosin production |
| CN101362924A (en) * | 2008-10-08 | 2009-02-11 | 中国林业科学研究院林产化学工业研究所 | Method for decolorization preparation of pale rosin by rosin containing non-decoloring agent |
| CN101649160A (en) * | 2009-09-11 | 2010-02-17 | 广西民族大学 | Method for producing refined light-color rosin by using turpentine as raw material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105086833A (en) * | 2015-09-29 | 2015-11-25 | 广西梧州日成林产化工股份有限公司 | Preparation method of polymerized rosin with high softening point |
| CN105860854A (en) * | 2016-05-13 | 2016-08-17 | 广西融水闽兴树脂有限公司 | Water-white rosin production line |
| CN106905855A (en) * | 2017-03-29 | 2017-06-30 | 南宁市青秀区嘉利林化有限公司 | The method that hydrogenated rosin is prepared from rosin |
| CN108789985A (en) * | 2018-04-28 | 2018-11-13 | 中国地质大学（北京） | Optimize the method and Chinese wax amber that Baltic amber prepares Chinese wax amber by heat |
| CN108789985B (en) * | 2018-04-28 | 2020-01-21 | 中国地质大学（北京） | Method for preparing white wax amber by thermally optimizing baltic sea amber and white wax amber |
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Application publication date: 20130724 |