CN103952179B - Special paper Wax special that a kind of montanin wax saponification is refining and preparation method thereof - Google Patents
Special paper Wax special that a kind of montanin wax saponification is refining and preparation method thereof Download PDFInfo
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- CN103952179B CN103952179B CN201410144719.2A CN201410144719A CN103952179B CN 103952179 B CN103952179 B CN 103952179B CN 201410144719 A CN201410144719 A CN 201410144719A CN 103952179 B CN103952179 B CN 103952179B
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Abstract
The invention discloses refining special paper Wax special of a kind of montanin wax saponification and preparation method thereof.The fusing point of described special paper Wax special is 90 ~ 100 DEG C, and penetration degree is 1 ~ 2, and acid number is 10 ~ 15mgKOH/g, and saponification value is 80 ~ 100mgKOH/g, and ash oontent is 1.2 ~ 2.5%, and resin content is 15 ~ 20%.First montanin wax 600 ~ 800kg and solvent is added reactor by the mass ratio of 1:1 ~ 3 and is heated to wax and dissolves by described preparation method, after insulated and stirred 10 ~ 30min, the aqueous solution 20 ~ 50kg of any one in alkali metal hydroxide, alkali metal hydrocarbonate or alkaline carbonate is added reactor, heated and stirred 2 ~ 3h reaches 10 ~ 15mgKOH/g to reactant acid number.The azeotrope that reaction is formed gets rid of waste water after condensation, separation, and the solvent in non-condensable gases is back to reactor in the lump with the solvent be separated after reclaiming, and continues to participate in reaction cycle.Described method production technique is simple, and equipment interoperability is good, and prepared special paper Wax special has good molten oil, fat dissolving, and sprawl levelling property and film-forming properties, the coat slurry formed has good mobility, and application value is higher.
Description
Technical field
The invention belongs to modified montan wax technical field, belong to montanin wax saponification technical field further, be specifically related to refining special paper Wax special of a kind of montanin wax saponification and preparation method thereof.
Background technology
China is one of brown coal reserves big country, the long-chain fat ester (wax ester) that the montanin wax extracted from brown coal is formed primarily of longer chain fatty acid (cerinic acid) and long chain aliphatic alcohol (ceryl alcohol), the free cerinic acid of part, the compositions such as small part ceryl alcohol, cerotone, aliphatic hydrocarbon, have the good characteristics such as fusing point is high, chemical stability good, physical strength is high, electroconductibility is low, moisture-proof.Because montanin wax derives from the organic compound of Coal-forming Plants, without carcinogenesis, thus obtain applying more and more widely in daily necessities, light industry, weaving, papermaking, printing and dyeing industry.The saponification of montanin wax is refined and is mainly utilized the lipid acid contained in wax under the effect of auxiliary agent, reacts, improves a series of physico-chemical properties of wax, meet the different demands of derived product with alkali-metal oxyhydroxide, carbonate or supercarbonate.On this basis, the present invention is intended to research and develop refining special paper Wax special of a kind of montanin wax saponification and preparation method thereof, by optimizing every processing condition of montanin wax saponification reaction, further to the molten oil of montanin wax, fat dissolving, sprawl levelling property and film-forming properties etc. to improve, produce the special paper Wax special goods of excellent property, improve the economic value added that montanin wax is produced further.
Summary of the invention
The first object of the present invention is the special paper Wax special providing a kind of montanin wax saponification refining; Second object is the preparation method providing described special paper Wax special.
The first object of the present invention is achieved in that the fusing point of the special paper Wax special that described montanin wax saponification is refined is 90 ~ 100 DEG C, and penetration degree is 1 ~ 2, acid number is 10 ~ 15mgKOH/g, saponification value is 80 ~ 100mgKOH/g, and ash oontent is 1.2 ~ 2.5%, and resin content is 15 ~ 20%.
The second object of the present invention is achieved in that the preparation method of the special paper Wax special that described montanin wax saponification is refined, and comprises dissolving, homogeneous, saponification and reflow process, specifically comprises:
A, dissolving: add in reactor by the mass ratio of 1:1 ~ 3 by montanin wax 600 ~ 800kg and solvent, be heated to montanin wax and dissolve;
B, homogeneous: open stirring rake, insulated and stirred 10 ~ 30min, to wax liquid and solvent even;
C, saponification: by any one the aqueous solution 20 ~ 50kg in alkali metal hydroxide, alkali metal hydrocarbonate or alkaline carbonate, slowly add in reactor, heated and stirred reaction 2 ~ 3h, until the acid number of reactant reaches 10 ~ 15mgKOH/g;
D, backflow: the azeotrope that solvent and the water produced in saponification reaction are formed is after condensation, being separated, get rid of waste water, solvent in non-condensable gases in condensation, sepn process, after reclaiming, is back to reactor in the lump with isolated solvent, continues to participate in reaction cycle.
The present invention is optimized from every processing condition of following several respects to montanin wax saponification reaction: solvent is selected, and the present invention is preferred toluene, as solvent and dewatering agent, has taken into account the volatility of solvent and the dissolution rate of wax; In the selection of saponifying agent, the alkaline carbonate selected by the present invention, supercarbonate have gentle response characteristic, and reaction controllability is strong, effectively improves the quality stability of finished product wax; Dissolve and saponification temperature selection on, temperature range set by the present invention ensure that the abundant dissolving of montanin wax on the one hand, more even with mixing of saponifying agent, avoid excessive temperature to cause the sex change of wax on the other hand, detrimentally affect is caused to the quality of finished product wax and yield; In the selection of auxiliary agent, the present invention can preferably add a small amount of polyoxyethylene glycol, utilizes it easily to form the feature of complex compound with alkalimetal ion, activity hydroxy in raising reaction system, carrying out smoothly of promotion saponification reaction; In the selection in reaction times, the reaction times set by the present invention has taken into account production efficiency, finished product wax yield and foreign matter content aspects factor, remarkable in economical benefits.In addition, the method of the invention raw material sources are extensive, production technique is simple, equipment interoperability is good, the special paper Wax special produced has good molten oil, fat dissolving, and sprawl levelling property and film-forming properties, the coat slurry formed has good mobility, steady quality is reliable, has higher application value.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet;
In figure: 1-reactor, 2-wax medial launder, 3-forming machine, 4-chemical feedstocks header tank, 5-catalyzer header tank, 6-additive header tank, 7-condenser, 8-water-and-oil separator, 9-device for absorbing tail gas.
Embodiment
The present invention is further illustrated below, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
The fusing point of the special paper Wax special that montanin wax saponification of the present invention is refined is 90 ~ 100 DEG C, and penetration degree is 1 ~ 2, and acid number is 10 ~ 15mgKOH/g, and saponification value is 80 ~ 100mgKOH/g, and ash oontent is 1.2 ~ 2.5%, and resin content is 15 ~ 20%.
The preparation method of the special paper Wax special that montanin wax saponification of the present invention is refined, comprises dissolving, homogeneous, saponification and reflow process, specifically comprises:
Described dissolving adds in reactor by montanin wax 600 ~ 800kg and solvent by the mass ratio of 1:1 ~ 3, is heated to montanin wax and dissolves;
Described homogeneous refers to unlatching stirring rake, insulated and stirred 10 ~ 30min, to wax liquid and solvent even;
Described saponification is by any one the aqueous solution 20 ~ 50kg in alkali metal hydroxide, alkali metal hydrocarbonate or alkaline carbonate, slowly adds in reactor, and heated and stirred reaction 2 ~ 3h, until the acid number of reactant reaches 10 ~ 15mgKOH/g;
Described backflow refers to azeotrope that solvent and the water produced in saponification reaction formed after condensation, being separated, get rid of waste water, solvent in non-condensable gases in condensation, sepn process, after reclaiming, is back to reactor in the lump with isolated solvent, continues to participate in reaction cycle.
In described dissolution process, the acid number of montanin wax is 30 ~ 50mgKOH/g.
The solvent used in described dissolution process can be any one in benzene, toluene or hexanaphthene.
The preferred toluene of described solvent.
Described dissolving final temperature is 90-100 DEG C, and described holding temperature is 90-100 DEG C, and described temperature of reaction is
105-120dEG C.
The basic metal used in described saponifying process can be any one in sodium or potassium.
The mass percent concentration of described alkali metal hydroxide aqueous solution is 30 ~ 50%, and the mass percent concentration of the alkali metal hydrocarbonate aqueous solution is 30 ~ 50%, and the mass percent concentration of aqueous alkali carbonate solution is 30 ~ 50%.
Described stirring velocity is 120 ~ 160r/min.
The beginning of described saponifying process, can also add polyoxyethylene glycol according to 3 ~ 4% of montanin wax quality.
Embodiment 1
Montanin wax 650kg and benzene are added in reactor by the mass ratio of 1:2, is heated to 90 ~ 94 DEG C gradually, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 25min of 150r/min, mix with benzene to wax liquid.Then the wet chemical 37kg of concentration 40% is slowly added in reactor, continue reflux in 105 ~ 110 DEG C with same rotating speed and stir 2.5h, until the acid number of reactant reaches 12mgKOH/g.The azeotrope that benzene and the water produced in saponification reaction are formed, after condensation, being separated, gets rid of waste water, and the benzene in the non-condensable gases in condensation, sepn process, after reclaiming, is back to reactor in the lump with isolated benzene, continues to participate in reaction cycle.
Embodiment 2
Montanin wax 700kg and hexanaphthene are added in reactor by the mass ratio of 1:3, is heated to 92 ~ 96 DEG C gradually, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 20min of 120r/min, mix with hexanaphthene to wax liquid.Then the aqueous sodium carbonate 33kg of concentration 40% is slowly added in reactor, continue reflux in 112 ~ 117 DEG C with same rotating speed and stir 2h, until the acid number of reactant reaches 10mgKOH/g.The azeotrope that hexanaphthene and the water produced in saponification reaction are formed is after condensation, being separated, get rid of waste water, hexanaphthene in non-condensable gases in condensation, sepn process, after reclaiming, is back to reactor in the lump with isolated hexanaphthene, continues to participate in reaction cycle.
Embodiment 3
Montanin wax 720kg and toluene are added in reactor by the mass ratio of 1:2, is heated to 95 ~ 98 DEG C gradually, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 30min of 140r/min, mix with toluene to wax liquid.Then the sodium bicarbonate aqueous solution 50kg of concentration 50% is slowly added in reactor, continue reflux in 110 ~ 118 DEG C with same rotating speed and stir 2.5h, until the acid number of reactant reaches 13mgKOH/g.The azeotrope that toluene and the water produced in saponification reaction are formed, after condensation, being separated, gets rid of waste water, and the toluene in the non-condensable gases in condensation, sepn process, after reclaiming, is back to reactor in the lump with isolated toluene, continues to participate in reaction cycle.
Embodiment 4
Montanin wax 600kg and toluene are added in reactor by the mass ratio of 1:1, is heated to 98 ~ 100 DEG C gradually, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 10min of 160r/min, mix with toluene to wax liquid.Then the aqueous sodium hydroxide solution 20kg of concentration 30% is slowly added in reactor, continue reflux in 114 ~ 120 DEG C with same rotating speed and stir 3h, until the acid number of reactant reaches 15mgKOH/g.The azeotrope that toluene and the water produced in saponification reaction are formed, after condensation, being separated, gets rid of waste water, and the toluene in the non-condensable gases in condensation, sepn process, after reclaiming, is back to reactor in the lump with isolated toluene, continues to participate in reaction cycle.
Embodiment 5
Montanin wax 800kg and benzene are added in reactor by the mass ratio of 1:3, is heated to 96 ~ 99 DEG C gradually, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 15min of 130r/min, mix with benzene to wax liquid.Then add polyoxyethylene glycol according to 3.5% of montanin wax quality, then the wet chemical 25kg of concentration 35% is slowly added in reactor, continue reflux in 107 ~ 115 DEG C with same rotating speed and stir 2h, until the acid number of reactant reaches 11mgKOH/g.The azeotrope that benzene and the water produced in saponification reaction are formed, after condensation, being separated, gets rid of waste water, and the benzene in the non-condensable gases in condensation, sepn process, after reclaiming, is back to reactor in the lump with isolated benzene, continues to participate in reaction cycle.
Claims (4)
1. the special paper Wax special that montanin wax saponification is refining, it is characterized in that the fusing point of described special paper Wax special is 90 ~ 100 DEG C, penetration degree is 1 ~ 2, acid number is 10 ~ 15mgKOH/g, saponification value is 80 ~ 100mgKOH/g, and ash oontent is 1.2 ~ 2.5%, and resin content is 15 ~ 20%; The preparation method of described special paper Wax special comprises dissolving, homogeneous, saponification and reflow process, specifically comprises:
A, dissolving: montanin wax 600 ~ 800kg and benzene, toluene or hexanaphthene are added in reactor by the mass ratio of 1:1 ~ 3, be heated to montanin wax and dissolve, dissolving final temperature is 90 ~ 100 DEG C;
B, homogeneous: open stirring rake, 90 ~ 100 DEG C of insulated and stirred 10 ~ 30min, to wax liquid and solvent even;
C, saponification: by any one the aqueous solution 20 ~ 50kg in alkali metal hydroxide, alkali metal hydrocarbonate or alkaline carbonate, described basic metal is sodium or potassium, slowly add in reactor, 105 ~ 120 DEG C of heated and stirred reaction 2 ~ 3h, until the acid number of reactant reaches 10 ~ 15mgKOH/g;
D, backflow: the azeotrope that solvent and the water produced in saponification reaction are formed is after condensation, being separated, get rid of waste water, solvent in non-condensable gases in condensation, sepn process, after reclaiming, is back to reactor in the lump with isolated solvent, continues to participate in reaction cycle.
2. the special paper Wax special that montanin wax saponification is refining according to claim 1, it is characterized in that the mass percent concentration of the alkali metal hydroxide aqueous solution described in step C is 30 ~ 50%, the mass percent concentration of the alkali metal hydrocarbonate aqueous solution is 30 ~ 50%, and the mass percent concentration of aqueous alkali carbonate solution is 30 ~ 50%.
3. the special paper Wax special that montanin wax saponification is refining according to claim 1, is characterized in that stirring velocity described in step B, C is 120 ~ 160r/min.
4. the special paper Wax special that montanin wax saponification is refining according to claim 1, adds polyoxyethylene glycol according to 3 ~ 4% of montanin wax quality when it is characterized in that the beginning of saponification reaction described in step C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410144719.2A CN103952179B (en) | 2014-04-12 | 2014-04-12 | Special paper Wax special that a kind of montanin wax saponification is refining and preparation method thereof |
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| CN201410144719.2A CN103952179B (en) | 2014-04-12 | 2014-04-12 | Special paper Wax special that a kind of montanin wax saponification is refining and preparation method thereof |
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| CN103952179B true CN103952179B (en) | 2015-12-02 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1185210A (en) * | 1966-12-23 | 1970-03-25 | Hoechst Ag | Process for preparing carbon paper waxes |
| CN101497817A (en) * | 2009-01-19 | 2009-08-05 | 李定忠 | Method for extracting wax in lignite |
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2014
- 2014-04-12 CN CN201410144719.2A patent/CN103952179B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1185210A (en) * | 1966-12-23 | 1970-03-25 | Hoechst Ag | Process for preparing carbon paper waxes |
| CN101497817A (en) * | 2009-01-19 | 2009-08-05 | 李定忠 | Method for extracting wax in lignite |
Non-Patent Citations (1)
| Title |
|---|
| "褐煤蜡的工业制备及精制技术";张声俊等;《化工进展》;20120531;第30卷;第509页第1栏倒数第1段-第2栏、第510页表1和表2、第512页第1.2.3节 * |
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