CN103881751A - Solvent-type wax saponified and refined from lignite wax and preparation method of solvent-type wax - Google Patents
Solvent-type wax saponified and refined from lignite wax and preparation method of solvent-type wax Download PDFInfo
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- CN103881751A CN103881751A CN201410144721.XA CN201410144721A CN103881751A CN 103881751 A CN103881751 A CN 103881751A CN 201410144721 A CN201410144721 A CN 201410144721A CN 103881751 A CN103881751 A CN 103881751A
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Abstract
The invention discloses a solvent-type wax saponified and refined from lignite wax and a preparation method of the solvent-type wax. The solvent-type wax has a melting point of 100-120 DEG C, a needle penetration of 1-2 and an acid value of 10-15mgKOH/g, a saponification value of 60-80mgKOH/g, an ash content of 1.2%-2.5% and a resin content of 20-25%. The preparation method comprises the steps of adding 600-800kg of lignite wax and a solvent according to a mass ratio of 1: (1-3) into a reaction kettle, heating until the wax is dissolved, carrying out heat preservation, stirring for 10-30 minutes, adding 5-10kg of any one of an alkaline earth metal oxide powder or hydroxide powder to the reaction kettle and stirring for 3-4 hours under heating until the acid value of the reactant is 10-15mgKOH/g, reacting to obtain an azeotrope, condensing the azeotrope, separating, discharging wastewater, recovering the solvent from the non-condensable gas to obtain the recovered solvent, and allowing the recovered solvent together with the separated solvent to be in backflow to the reaction kettle to continue the reaction. The method disclosed by the invention is simple, equipment has good versatility, the solvent-type wax prepared by the method disclosed by the invention has high hardness and strength, good affinity to solvents and oils, capability of being condensed into a hard and delicate, smooth and bright hard paste, good wipe brightness and is free of dialysis and separation of solvent and particularly suitable for the production of starting materials of a solvent-containing decorating agent and a polish.
Description
Technical field
The invention belongs to modified montan wax technical field, further belong to montanin wax saponification technical field, be specifically related to refining solvent-borne type wax 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 extracting from brown coal is mainly made up 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, thereby obtain applying more and more widely in daily necessities, light industry, weaving, papermaking, printing and dyeing industry.It is mainly to utilize the lipid acid containing in wax under the effect of auxiliary agent that the saponification of montanin wax is refined, and reacts with oxide compound or the oxyhydroxide of alkaline-earth metal, improves a series of physico-chemical properties of wax, meets the different demands of derived product.On this basis, the present invention is intended to research and develop refining solvent-borne type wax of a kind of montanin wax saponification and preparation method thereof, by optimizing every processing condition of montanin wax saponification reaction, further modification is carried out in the hardness to montanin wax, solvent absorbing ability and slip effect, produce the solvent-borne type wax work of excellent property, further improve the economic value added that montanin wax is produced.
Summary of the invention
The solvent-borne type wax that provides a kind of montanin wax saponification refining is provided the first object of the present invention; The second object is to provide the preparation method of described solvent-borne type wax.
The first object of the present invention is achieved in that the fusing point of the refining solvent-borne type wax of described montanin wax saponification is 100 ~ 120 ℃, and penetration degree is 1 ~ 2, acid number is 10 ~ 15mgKOH/g, saponification value is 60 ~ 80mgKOH/g, and ash oontent is 1.2 ~ 2.5%, and resin content is 20 ~ 25%.
The second object of the present invention is achieved in that the preparation method of the refining solvent-borne type wax of described montanin wax saponification, comprises dissolving, homogeneous, saponification and reflow process, specifically comprises:
A, dissolving: montanin wax 600 ~ 800kg and solvent are added in reactor by the mass ratio of 1:1 ~ 3, be heated to montanin wax and dissolve;
B, homogeneous: open stirring rake, insulated and stirred 10 ~ 30min, even to wax liquid and solvent;
C, saponification: by any powder 5 ~ 10kg in alkaline earth metal oxide or oxyhydroxide, slowly add in reactor, heated and stirred reaction 3 ~ 4h, until the acid number of reactant reaches 10 ~ 15mgKOH/g;
D, backflow: the azeotrope that solvent forms with the water producing in saponification reaction is after condensation, separating, 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 every processing condition of montanin wax saponification reaction from following several respects: solvent is selected, the present invention is preferred toluene, dimethylbenzene, as solvent, has been taken into account the volatility of solvent and the dissolution rate of wax; In the selection of alkaline matter, the present invention has selected the oxyhydroxide of alkaline-earth metal and oxide compound as saponifying agent, makes reaction more steadily controlled; In the selection of dissolving and saponification temperature, the temperature range that the present invention sets has guaranteed the abundant dissolving of montanin wax on the one hand, more even with mixing of saponifying agent, avoid on the other hand excessive temperature to cause the sex change of wax, quality and yield to finished product wax cause detrimentally affect; In the selection of saponification time, the reaction times that the present invention sets can guarantee that the lipid acid in montanin wax fully reacts with alkaline matter, is conducive to carrying out smoothly of saponification reaction, has improved the yield of finished product solvent-borne type wax, 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 solvent-borne type wax hardness of producing is high, intensity is large, solvent and oil are had to good avidity, more more excellent than the carnauba wax that is known as the king in wax, can be dissolved in 4 ~ 6 times of hot organic solvents (as turps or industrial naptha), coagulable is that structure is very hard, fine and smooth, the bright plaster body of surfacing, and have and well wipe luminance brightness, there is not the phenomenons such as any solvent dialysis separation, be particularly suitable for producing the initial feed of solvent-laden decorations and polishing material, application value is higher.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention;
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 never in any form the present invention is limited, and any conversion or the replacement done based on training centre of the present invention, all belong to protection scope of the present invention.
The fusing point of the refining solvent-borne type wax of montanin wax saponification of the present invention is 100 ~ 120 ℃, and penetration degree is 1 ~ 2, and acid number is 10 ~ 15mgKOH/g, and saponification value is 60 ~ 80mgKOH/g, and ash oontent is 1.2 ~ 2.5%, and resin content is 20 ~ 25%.
The preparation method of the refining solvent-borne type wax of montanin wax saponification of the present invention, comprises dissolving, homogeneous, saponification and reflow process, specifically comprises:
Described dissolving is that montanin wax 600 ~ 800kg and solvent are added in reactor by the mass ratio of 1:1 ~ 3, is heated to montanin wax and dissolves;
Described homogeneous refers to unlatching stirring rake, and insulated and stirred 10 ~ 30min is even to wax liquid and solvent;
Described saponification is by any powder 5 ~ 10kg in alkaline earth metal oxide or oxyhydroxide, slowly adds in reactor, and heated and stirred reaction 3 ~ 4h, until the acid number of reactant reaches 10 ~ 15mgKOH/g;
Described backflow refers to azeotrope that solvent forms with the water that produces in saponification reaction after condensation, separating, 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 using in described dissolution process can be any in benzene, toluene, hexanaphthene.
Described solvent is preferably toluene.
Described dissolving final temperature is 90 ~ 100 ℃, and described holding temperature is 90 ~ 100 ℃, and described temperature of reaction is 115-125 ℃.
The alkaline-earth metal using in described saponifying process refers to any in calcium, magnesium or barium.
Particle diameter≤150 μ the m of described alkaline earth metal oxide or hydroxide powder.
Described stirring velocity is 120 ~ 160r/min.
embodiment 1
Montanin wax 700kg and toluene are added in reactor by the mass ratio of 1:2, be heated to gradually 93 ~ 97 ℃, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 20min of 140r/min, mix with toluene to wax liquid.Then the calcium hydroxide powder 7.8kg of 120 μ m is slowly added in reactor, continue reflux in 118 ~ 122 ℃ with same rotating speed and stir 3.5h, until the acid number of reactant reaches 12mgKOH/g.The azeotrope that toluene forms with the water producing in saponification reaction, after condensation, separating, is got 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.
Montanin wax 800kg and hexanaphthene are added in reactor by the mass ratio of 1:3, be heated to gradually 93 ~ 95 ℃, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 10min of 120r/min, mix with hexanaphthene to wax liquid.Then the lime powder 8.5kg of 60 μ m is slowly added in reactor, continue reflux in 115 ~ 120 ℃ with same rotating speed and stir 3h, until the acid number of reactant reaches 10mgKOH/g.The azeotrope that hexanaphthene forms with the water producing in saponification reaction is after condensation, separating, 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.
Montanin wax 600kg and toluene are added in reactor by the mass ratio of 1:1, be heated to gradually 90 ~ 92 ℃, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 30min of 160r/min, mix with toluene to wax liquid.Then the magnesium oxide powder 9.3kg of 150 μ m is slowly added in reactor, continue reflux in 120 ~ 125 ℃ with same rotating speed and stir 4h, until the acid number of reactant reaches 15mgKOH/g.The azeotrope that toluene forms with the water producing in saponification reaction, after condensation, separating, is got 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.
Montanin wax 650kg and toluene are added in reactor by the mass ratio of 1:1.5, be heated to gradually 95 ~ 99 ℃, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 15min of 150r/min, mix with toluene to wax liquid.Then the barium oxide powder 5kg of 80 μ m is slowly added in reactor, continue reflux in 115 ~ 119 ℃ with same rotating speed and stir 4h, until the acid number of reactant reaches 14mgKOH/g.The azeotrope that toluene forms with the water producing in saponification reaction, after condensation, separating, is got 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 750kg and benzene are added in reactor by the mass ratio of 1:2.5, be heated to gradually 97 ~ 100 ℃, treat that montanin wax fully dissolves.Then open stirring rake, with the speed insulated and stirred 25min of 130r/min, mix with benzene to wax liquid.Then the calcium hydroxide powder 10kg of 110 μ m is slowly added in reactor, continue reflux in 118 ~ 124 ℃ with same rotating speed and stir 3.5h, until the acid number of reactant reaches 11mgKOH/g.The azeotrope that benzene forms with the water producing in saponification reaction, after condensation, separating, is got 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 (8)
1. the refining solvent-borne type wax of montanin wax saponification, the fusing point that it is characterized in that described solvent-borne type wax is 100 ~ 120 ℃, penetration degree is 1 ~ 2, acid number is 10 ~ 15mgKOH/g, saponification value is 60 ~ 80mgKOH/g, and ash oontent is 1.2 ~ 2.5%, and resin content is 20 ~ 25%.
2. a preparation method for the refining solvent-borne type wax of montanin wax saponification according to claim 1, is characterized in that comprising dissolving, homogeneous, saponification and reflow process, specifically comprises:
A, dissolving: montanin wax 600 ~ 800kg and solvent are added in reactor by the mass ratio of 1:1 ~ 3, be heated to montanin wax and dissolve;
B, homogeneous: open stirring rake, insulated and stirred 10 ~ 30min, even to wax liquid and solvent;
C, saponification: by any powder 5 ~ 10kg in alkaline earth metal oxide or oxyhydroxide, slowly add in reactor, heated and stirred reaction 3 ~ 4h, until the acid number of reactant reaches 10 ~ 15mgKOH/g;
D, backflow: the azeotrope that solvent forms with the water producing in saponification reaction is after condensation, separating, 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.
3. preparation method according to claim 2, is characterized in that solvent described in steps A can be any in benzene, toluene or hexanaphthene.
4. preparation method according to claim 3, is characterized in that described solvent is toluene.
5. preparation method according to claim 2, is characterized in that alkaline-earth metal described in step C refers to any in calcium, magnesium or barium.
6. preparation method according to claim 2, is characterized in that alkaline earth metal oxide described in step C or the particle diameter≤150 μ m of hydroxide powder.
7. preparation method according to claim 2, is characterized in that the dissolving final temperature described in steps A is 90 ~ 100 ℃, and the holding temperature described in step B is 90 ~ 100 ℃, and the temperature of reaction described in step C is 115 ~ 125 ℃.
8. preparation method according to claim 2, is characterized in that the stirring velocity described in step B and step C is 120 ~ 160r/min.
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| CN201410144721.XA CN103881751B (en) | 2014-04-12 | 2014-04-12 | Solvent-borne type wax that a kind of montanin wax saponification is refining and preparation method thereof |
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| CN201410144721.XA CN103881751B (en) | 2014-04-12 | 2014-04-12 | Solvent-borne type wax that a kind of montanin wax saponification is refining and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108191602A (en) * | 2018-01-02 | 2018-06-22 | 重庆合才化工有限公司 | A kind of rice bran cerinic acid calcium soap wax and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936510A (en) * | 2012-10-26 | 2013-02-20 | 安徽工业大学 | Method for extracting higher aliphatic compound from lignite |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936510A (en) * | 2012-10-26 | 2013-02-20 | 安徽工业大学 | Method for extracting higher aliphatic compound from lignite |
Non-Patent Citations (2)
| Title |
|---|
| 张声俊等: "褐煤蜡的工业制备及精制技术", 《化工进展》, vol. 30, 31 December 2011 (2011-12-31), pages 509 - 513 * |
| 戴和武等: "《褐煤利用技术》", 28 February 1999, 煤炭工业出版社, article "褐煤蜡", pages: 351-361 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108191602A (en) * | 2018-01-02 | 2018-06-22 | 重庆合才化工有限公司 | A kind of rice bran cerinic acid calcium soap wax and preparation method thereof |
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