CN103074108A - Degreasing method of crude montan wax - Google Patents
Degreasing method of crude montan wax Download PDFInfo
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- CN103074108A CN103074108A CN2012105225286A CN201210522528A CN103074108A CN 103074108 A CN103074108 A CN 103074108A CN 2012105225286 A CN2012105225286 A CN 2012105225286A CN 201210522528 A CN201210522528 A CN 201210522528A CN 103074108 A CN103074108 A CN 103074108A
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Abstract
The invention relates to a refining method of montan wax, and belongs to the technical field of the coal chemical engineering and the fine chemical engineering. The method for producing degreased montan wax by extracting resin impurities from crude montan wax treated as a raw material through a small-molecular-weight ester solvent sequentially comprises the following steps: 1, adding the crude montan wax and the small-molecular-weight ester solvent to a reactor according to a solid-liquid ratio of 1:3-6, and carrying out primary extraction at 70-125DEG C under a stirring condition for 2-4h; 2, cooling extracts obtained in step 1 to room temperature, and carrying out filtering separation to obtain a degreased filter cake and a resin-containing filtrate; 3, adding the degreased filter cake to the small-molecular-weight ester solvent, and carrying out secondary extraction at 70-125DEG C under a stirring condition to obtain a degreased filter cake and a resin-containing filtrate; and 4, carrying out normal or reduced pressure distillation of the degreased filtrate obtained in step 3 to recover the solvent and obtain the degreased montan wax, wherein a montan resin is a byproduct. The method has the advantages of small solvent application amount and reasonable technology.
Description
Technical field
The present invention relates to a kind of process for purification of montanin wax, belong to Coal Chemical Industry, fine chemical technology field.
Technical background
Generally all contain more resene impurity in the crude montan wax, the resin content of domestic crude montan wax is general all 20～30%.The resin of high-content can cause the Chemicals that contain this waxy stone to be clamminess, and has hindered it in the use of being permitted the utility wax industrial sector.In addition, in developing the various processing waxes take montanin wax as the basis, refining wax process, resin also is a kind of harmful impurity, needs be removed in advance.
About the degreasing method of crude montan wax, the earliest be superheated vapour vacuum distillation method and oxygenolysis method.What study at present more and industrial application is solvent extration, such as benzene solvent crystallisation by cooling method, cold benzene leaching method, ethyl acetate room temperature leaching method etc.Benzene solvent crystallisation by cooling method has the advantage that technique is simple, yield is high; But it exists solvent toxicity large and be difficult to the problem of filtering and washing because partial crystallization is material that colloidal causes.Cold benzene leaching method solid-liquid separation comparatively easily but it exists solvent toxicity large and need raw material is crushed in advance problem of fine particle and is prone to that raw material is softening, the phenomenon of adhesion when broken.Although ethyl acetate room temperature leaching method technique is simple, toxicity is low, its one way extraction efficiency is low, extraction is with duration and need repeatedly repeatedly extraction.
Summary of the invention
The object of the invention is to for deficiency of the prior art, the method for the crude montan wax degreasing that a kind of technique is reasonable, solvent load is few, raw material subject range is wide, quality product is high is provided.
The invention provides a kind of method of crude montan wax degreasing, a kind of take crude montan wax as raw material, remove resene impurity in the crude montan wax by the extraction of small molecular weight esters solvent, prepare the production method of degreasing montanin wax, comprise the step of following order:
A. the proportioning by solid-to-liquid ratio 1:3～6 adds crude montan wax and small molecular weight esters solvent in reactor, extracts 2～4 hours at 70～125 ℃ with agitation condition next time;
B. will extract material and be cooled to room temperature, and adopt the filtering separation mode to obtain degreasing filter cake and resiniferous filtrate;
C will take off. and the fat filter cake adds the small molecular weight esters solvent again, reextraction obtains under 70～125 ℃ and agitation condition degreasing filter cake and resiniferous filtrate;
D. with degreasing filtrate normal pressure or vacuum distillation recovered solvent, obtain the degreasing montanin wax, and the by-product valchovite.
The described crude montan wax raw material of step a is the chocolate sheet, need not break process.
The described small molecular weight esters solvent of step a, c is ethyl acetate or butylacetate; Wherein the temperature of reaction of ethyl acetate is 70～80 ℃, and the temperature of reaction of butylacetate is 70～125 ℃.
The described room temperature of step b is 15～25 ℃.
The solvent load of the described secondary solvent of step c extraction 0.65～1.0 times of solvent load when extracting for the first time, extraction time is 2～4 hours.
The present invention removes resene impurity in the crude montan wax by the extraction of small molecular weight esters solvent, preparation degreasing montanin wax, the method adopts ethyl acetate or butylacetate under the certain temperature condition crude montan wax to be carried out solvent extraction, extraction is chilled to room temperature after finishing, be separated by filtration and obtain degreasing filter cake and resiniferous filtrate, and then after solvent is reclaimed in boiling, namely get degreasing montanin wax product and valchovite.Whole technological process method solvent load is few, and technique is reasonable, raw material subject range is wide, quality product is high.
Embodiment
Embodiment 1
A, add resinous 27.86% crude montan wax 1000 grams and 4000 gram technical grade ethyl acetate in the extraction reactor, be heated to 72 ℃, extraction is 3 hours under stirring state.
B, material is cooled to room temperature, continues at ambient temperature to stir 0.5 hour.Then adopt the press filtration mode to carry out solid-liquid separation.Resiniferous liquid phase gets rosin products after the Distillation recovery ethyl acetate, filter cake is then dropped into again carries out reextraction in the extraction reactor.
C, add filter cake and 3000 gram technical grade ethyl acetate in the extraction reactor, be heated to 72 ℃, extraction is 3 hours under stirring state.
D, material is cooled to room temperature, continues at ambient temperature to stir 0.5 hour.Then adopt the press filtration mode to carry out solid-liquid separation.Resiniferous liquid phase after the Distillation recovery ethyl acetate rosin products, filter cake be-26 in vacuum tightness ~-the 30Kpa condition under vacuum distilling must the defatted wax product after reclaiming ethyl acetate.Final resin content 6.11%.
Embodiment 2
A, add resinous 27.86% 1000 gram crude montan waxs and 3000 gram technical grade butylacetates in the extraction reactor, be heated to 100 ℃, extraction is 3 hours under stirring state.
B, material is cooled to room temperature, continues at ambient temperature to stir 0.5 hour.Then adopt the press filtration mode to carry out solid-liquid separation.Resiniferous liquid phase gets rosin products behind the Distillation recovery butylacetate, filter cake is then dropped into again carries out reextraction in the extraction reactor.
C, add filter cake and 2200 gram technical grade ethyl acetate in the extraction reactor, be heated to 100 ℃, extraction is 3 hours under stirring state.
D, material is cooled to room temperature, continues at ambient temperature to stir 0.5 hour.Then adopt the press filtration mode to carry out solid-liquid separation.Resiniferous liquid phase behind the Distillation recovery butylacetate rosin products, filter cake be-50 in vacuum tightness ~-condition of 55Kpa under vacuum distilling reclaim behind the butylacetate must the defatted wax product, final resin content 5.73%.
Embodiment 3
A, add resinous 27.86% crude montan wax 800 grams and 3000 gram technical grade butylacetates in the extraction reactor, be heated to 80 ℃, extraction is 3 hours under stirring state.
B, material is cooled to room temperature, continues at ambient temperature to stir 0.5 hour.Then adopt the press filtration mode to carry out solid-liquid separation.Resiniferous liquid phase gets rosin products behind the Distillation recovery butylacetate, filter cake is then dropped into again carries out reextraction in the extraction reactor.
C, add filter cake and 2000 gram technical grade butylacetates in the extraction reactor, be heated to 80 ℃, extraction is 3 hours under stirring state.
D, material is cooled to room temperature, continues at ambient temperature to stir 0.5 hour.Then adopt the press filtration mode to carry out solid-liquid separation.Resiniferous liquid phase behind the Distillation recovery butylacetate rosin products, filter cake be-50 in vacuum tightness ~-condition of 55Kpa under, vacuum distilling is reclaimed behind the butylacetate must the defatted wax product, final resin content 5.16%.
Claims (5)
1. one kind take crude montan wax as raw material, removes resene impurity in the crude montan wax by the extraction of small molecular weight esters solvent, and the production method of preparation degreasing montanin wax comprises the step of following order:
A. the proportioning by solid-to-liquid ratio 1:3～6 adds crude montan wax and small molecular weight esters solvent in reactor, extracts 2～4 hours at 70～125 ℃ with agitation condition next time;
B. will extract material and be cooled to room temperature, and adopt the filtering separation mode to obtain degreasing filter cake and resiniferous filtrate;
C. the degreasing filter cake is added the small molecular weight esters solvent again, reextraction obtains under 70～125 ℃ and agitation condition degreasing filter cake and resiniferous filtrate;
D. with degreasing filtrate normal pressure or vacuum distillation recovered solvent, obtain the degreasing montanin wax, and the by-product valchovite.
2. require 1 described a kind of degreasing montanin wax production method according to the right item, wherein the described crude montan wax raw material of step a is the chocolate sheet, need not break process.
3. require 1 described a kind of degreasing montanin wax production method according to the right item, wherein the described small molecular weight esters solvent of step a, c is ethyl acetate or butylacetate; Wherein the temperature of reaction of ethyl acetate is 70～80 ℃, and the temperature of reaction of butylacetate is 70～125 ℃.
4. require 1 described a kind of degreasing montanin wax production method according to the right item, wherein the described room temperature of step b is 15～25 ℃.
5. require 1 described degreasing montanin wax production method according to the right item, the solvent load of the described secondary solvent of step c extraction 0.65～1.0 times of solvent load when extracting for the first time wherein, extraction time is 2～4 hours.
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| CN2012105225286A CN103074108A (en) | 2012-12-07 | 2012-12-07 | Degreasing method of crude montan wax |
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| CN2012105225286A CN103074108A (en) | 2012-12-07 | 2012-12-07 | Degreasing method of crude montan wax |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103614161A (en) * | 2013-12-04 | 2014-03-05 | 曲靖众一精细化工股份有限公司 | Efficient lignite wax deresination device and deresination method |
| CN104312627A (en) * | 2014-10-27 | 2015-01-28 | 中国矿业大学 | Solvent and method for removing resin from lignite wax by virtue of crystallization process |
| CN109913267A (en) * | 2017-12-12 | 2019-06-21 | 神华集团有限责任公司 | A kind of method of lignite dehydration co-production resin and lignite wax |
| CN109913268A (en) * | 2017-12-12 | 2019-06-21 | 神华集团有限责任公司 | By the method for lignite coproduction resin and lignite wax |
| CN110355180A (en) * | 2019-07-02 | 2019-10-22 | 国家能源集团宁夏煤业有限责任公司 | Wax residue treatment method and system |
| CN111154512A (en) * | 2018-11-08 | 2020-05-15 | 国家能源投资集团有限责任公司 | Method for removing resin from lignite crude wax and method for extracting lignite wax from lignite |
| CN113403107A (en) * | 2020-03-17 | 2021-09-17 | 国家能源投资集团有限责任公司 | Method for removing resin from coarse lignite wax |
Citations (1)
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| CN101402899A (en) * | 2008-11-17 | 2009-04-08 | 昆明理工大学 | Oxidization fine purification albefaction method for montan wax |
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2012
- 2012-12-07 CN CN2012105225286A patent/CN103074108A/en active Pending
Patent Citations (1)
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| CN101402899A (en) * | 2008-11-17 | 2009-04-08 | 昆明理工大学 | Oxidization fine purification albefaction method for montan wax |
Non-Patent Citations (1)
| Title |
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| 李宝才 等: "云南褐煤蜡氧化精制的研究", 《燃料化学学报》, vol. 27, no. 3, 30 June 1999 (1999-06-30) * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103614161A (en) * | 2013-12-04 | 2014-03-05 | 曲靖众一精细化工股份有限公司 | Efficient lignite wax deresination device and deresination method |
| CN103614161B (en) * | 2013-12-04 | 2015-04-01 | 曲靖众一精细化工股份有限公司 | Efficient lignite wax deresination device and deresination method |
| CN104312627A (en) * | 2014-10-27 | 2015-01-28 | 中国矿业大学 | Solvent and method for removing resin from lignite wax by virtue of crystallization process |
| CN104312627B (en) * | 2014-10-27 | 2016-03-02 | 中国矿业大学 | A kind of crystallization process removes solvent and the method for resin in montanin wax |
| CN109913267A (en) * | 2017-12-12 | 2019-06-21 | 神华集团有限责任公司 | A kind of method of lignite dehydration co-production resin and lignite wax |
| CN109913268A (en) * | 2017-12-12 | 2019-06-21 | 神华集团有限责任公司 | By the method for lignite coproduction resin and lignite wax |
| CN109913268B (en) * | 2017-12-12 | 2021-03-16 | 神华集团有限责任公司 | Method for co-producing resin and montan wax from lignite |
| CN109913267B (en) * | 2017-12-12 | 2021-03-30 | 神华集团有限责任公司 | Method for dehydrating lignite and co-producing resin and montan wax |
| CN111154512A (en) * | 2018-11-08 | 2020-05-15 | 国家能源投资集团有限责任公司 | Method for removing resin from lignite crude wax and method for extracting lignite wax from lignite |
| CN110355180A (en) * | 2019-07-02 | 2019-10-22 | 国家能源集团宁夏煤业有限责任公司 | Wax residue treatment method and system |
| CN113403107A (en) * | 2020-03-17 | 2021-09-17 | 国家能源投资集团有限责任公司 | Method for removing resin from coarse lignite wax |
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Application publication date: 20130501 |