CN101671574B - Production process of montan wax - Google Patents
Production process of montan wax Download PDFInfo
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- CN101671574B CN101671574B CN200910174277A CN200910174277A CN101671574B CN 101671574 B CN101671574 B CN 101671574B CN 200910174277 A CN200910174277 A CN 200910174277A CN 200910174277 A CN200910174277 A CN 200910174277A CN 101671574 B CN101671574 B CN 101671574B
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Abstract
The invention discloses a production process of montan wax, adopting mixed solvent of cyclohexane and alcohol. The production process comprises the following steps: smashing and screening lignite, putting coal particles of lignite into an extraction tank, putting mixed solvent in a volume ratio of solid to liquid of 1:1 to 1:4 for extraction and flash evaporating the extracted solution to recover the solvent; evaporating residual mixed solvent by a stewing system to obtain crude montan wax; vapor condensing the evaporated mixed solvent by a heat exchanger, then separating oil and water, and feeding upper-layer cyclohexane to a solvent feed tank; and separating tertiary butanol in lower-layer liquid from water by a rectification method, and introducing the separated tertiary butanol into the solvent feed tank; detecting the content of cyclohexane or tertiary butanol in the solvent feed tank, supplementing pure cyclohexane solvent and pure tertiary butanol solvent to lead the proportion of the two solvents to meet requirements, and then using the two solvents continuously. The extraction solvents of the production process have safety and reliability, simple extraction process, high wax yield, economy and environment protection, high reuse rate of solvents and low cost, thereby having wide practicability.
Description
The application divides an application for " montanin wax extraction solvent and production technique " application, and its applying date is: 2007.2.1; Application number is: 200710019959.X.
Technical field
The present invention relates to a kind of production process of montan wax.
Background technology
Montanin wax generally is meant the mixture of a kind of complex compound that brown coal obtain through organic solvent extraction.Montanin wax and fabricated product thereof are that present any natural wax or synthetic wax are irreplaceable, are a kind of indispensable important Chemicals in the present national economy.For the solvent of montanin wax extraction usefulness, the eighties adopts toluene in the world, adopts which kind of solvent at present because technical know-how is unknown.Domestic montanin wax enterprise (mainly containing Inner Mongol crow Dan Lachang, Yunnan Xun Dian wax factory) is employed then to be conventional organic solvents benzene always, and there is following problems in this solvent:
(1) benzene belongs to inflammable, explosive, poisonous objectionable impurities, and extraction process is again under near the comparatively high temps of its boiling point, to operate, and volatile quantity is big, and is very big to the harm of operator's health and surrounding environment;
(2) benzene is not ideal to the selectivity of wax, and resin and pitch earth content are higher in the montanin wax that is extracted, and the waxy stone quality of extraction is lower;
(3) remain in the use field that the benzene solvent in the montanin wax has limited product.
Summary of the invention
The objective of the invention is to overcome the weak point in the prior art, a kind of harm that reduces operator's health and surrounding environment be provided, extract of high grade, the production process of montan wax that use range is wide.
Montanin wax extracting production process of the present invention is:
A. brown coal are carried out fragmentation, screening, get the brown coal that grain diameter is 0.6～20mm;
B. the brown coal grain that screening is obtained is put into extractor, and adding the solid-liquid volume ratio is 1: 1～1: 4 the hexanaphthene and the mixed solvent of alcohols, extracts with saturated vapor heating, normal pressure or pressurization;
C. the solution after will extracting carries out flash distillation through vapo(u)rization system, reclaims mixed solvent, through decoction system remaining mixed solvent is evaporated again, promptly obtains the product montanin wax;
D. with the mixed solvent vapor condensation of interchanger with evaporation, carry out oily water separation then, several alkane of the ring on upper strata are sent into the mixed solvent storage tank, lower layer of water is carried out alcohol and the separating of water through rectifying tower, and isolating alcohol imports the mixed solvent storage tank;
E. detect several alkane of ring or pure content in the solvent feed tank, replenish several alkane of pure ring and alcoholic solvent respectively, after making it to meet ratio, deliver to again and continue in the extractor to use.
The invention has the beneficial effects as follows:
(1) hexanaphthene that is adopted and the synergistic effect of pure mixed solvent make that product wax rate is higher;
(2) good product quality, the wax color of extracting more shallow than benzene wax; Resin and pitch earth content are obviously lower;
(3) hexanaphthene and pure mixed solvent toxicity are little, help the improvement of operating environment and surrounding environment;
(4) not containing toxic substances such as benzene in the gained montanin wax, is environmentally friendly machine, will receive the welcome of its derived product producer, and may widen the Application Areas of montanin wax;
(5) hexanaphthene is lower than benzene with pure mixed solvent boiling point; The benzene boiling point is 82 ℃; Hexanaphthene is 62～74 ℃ (relevant with the proportioning of mixed solvent) with pure mixed solvent boiling point; The heat energy that hexanaphthene and pure mixed solvent need is less, and it is low to consume energy, and generally under near the temperature of boiling point, carries out just obtaining the bigger wax rate of putting forward during extraction;
(6) do not increase cost.Hexanaphthene and pure mixed solvent repeat usage are high, and price is suitable with the coking benzene price.
Adopt same even coal sample, adopt benzene and mixed extractant solvent montanin wax of the present invention respectively, the average comparison of test results of each item index is following:
Table 1
Description of drawings
Accompanying drawing is the technological process of production figure of montanin wax extraction solvent of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are done further to describe:
The mixed extractant solvent montanin wax of enforcement one, the employing trimethyl carbinol and hexanaphthene, the mass percent of mixed solvent: hexanaphthene is 60%, the trimethyl carbinol (methyl alcohol or ethanol) is 40%.
The technological process of production at first gets into coal grain storehouse with the raw material brown coal with crusher in crushing, bolting shown in accompanying drawing, get the brown coal of grain diameter 1～10mm; 1 ton of brown coal is put into chuck heating-type extractor, is that 1: 2.5 ratio is put into 2.3m in the solid-liquid volume ratio
3The mixed uniformly trimethyl carbinol (methyl alcohol or ethanol) and hexanaphthene mixed solvent extract, and with 120 ℃ of saturated vapor heating, red-tape operati pressure is between 3～4MPa, and pressure is above promptly stopping heating, and hypotony then reheats, 2 hours extraction time; Solution after the extraction with being pumped into flash distillation in the vapo(u)rization system, reclaiming the trimethyl carbinol (methyl alcohol or ethanol) and hexanaphthene mixed solvent, is evaporated remaining mixed solvent through decoction system again, promptly obtain montanin wax, use the shaper extrusion molding.Use the shell and tube heat exchanger heat exchange; With water is condensing agent; Behind the mixed solvent vapor condensation of collecting in vapo(u)rization system and the decoction system, to send in the water-and-oil separator and separate, the hexanaphthene liquid on the upper strata gets into the mixed solvent storage tank; After the trimethyl carbinol in lower floor's liquid (methyl alcohol or ethanol) got into rectifying tower and water sepn, isolated water got into wastewater disposal basin and fully utilizes; The isolated trimethyl carbinol (methyl alcohol or ethanol) gets into the mixed solvent storage tank, can continue to use with getting into hexanaphthene.The mixed solvent that reclaims is about 1.8m
3, detect the content that encircles several alkane or the trimethyl carbinol (methyl alcohol or ethanol) in the mixed solvent storage tank before using earlier, replenish two kinds of neat solvents respectively in the mixed solvent storage tank, several alkane of ring and the trimethyl carbinol (methyl alcohol or ethanol) mass ratio were remained 60%: 40%.
Embodiment two, mixed solvent prescription: encircling several alkane and the trimethyl carbinol (methyl alcohol or ethanol) mass percent is 80%: 20%.Its production technique and embodiment one are basic identical, and different is: adopting the pot group type extraction, is one group with three jars, the solvent counter-current operation.Detailed process is: several alkane of fresh ring and the trimethyl carbinol (methyl alcohol or ethanol) mixed solvent are sent in the extractor that wherein brown coal be extracted twice; With the condition identical with embodiment one; Extract the brown coal of sending into again after 1 hour wherein and be extracted in the extractor once, more not stripped brown coal are extracted.Discharging renewed coal after brown coal were extracted three times, carried out successively.
Claims (1)
1. production process of montan wax is characterized in that:
A. brown coal are carried out fragmentation, screening, get the brown coal that grain diameter is 0.6～20mm;
B. the brown coal grain that screening is obtained is put into extractor, and adding the solid-liquid volume ratio is 1: 1～1: 4 the hexanaphthene and the mixed solvent of alcohols, extracts with saturated vapor heating, normal pressure or pressurization;
C. the solution after will extracting carries out flash distillation through vapo(u)rization system, reclaims mixed solvent, through decoction system remaining mixed solvent is evaporated again, promptly obtains the product montanin wax;
D. with the mixed solvent vapor condensation of interchanger with evaporation, carry out oily water separation then, the hexanaphthene on upper strata is sent into the mixed solvent storage tank, lower layer of water is carried out alcohol and the separating of water through rectifying tower, and isolating alcohol imports the mixed solvent storage tank;
E. detect hexanaphthene or pure content in the solvent feed tank, replenish pure hexanaphthene and alcoholic solvent respectively, make it to meet the mass ratio of mixed solvent: hexanaphthene is 30-90%, and alcohols is 70-10%, delivers to and continues in the extractor to use; Said alcohols is the trimethyl carbinol, methyl alcohol or ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910174277A CN101671574B (en) | 2007-02-01 | 2007-02-01 | Production process of montan wax |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910174277A CN101671574B (en) | 2007-02-01 | 2007-02-01 | Production process of montan wax |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200710019959A Division CN101029255B (en) | 2007-02-01 | 2007-02-01 | Brown-coal green extractive solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101671574A CN101671574A (en) | 2010-03-17 |
| CN101671574B true CN101671574B (en) | 2012-10-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200910174277A Expired - Fee Related CN101671574B (en) | 2007-02-01 | 2007-02-01 | Production process of montan wax |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899089B (en) * | 2012-09-11 | 2014-08-20 | 国电燃料有限公司 | Production process for soft montan wax |
| CN103074109B (en) * | 2013-02-06 | 2015-03-18 | 云南尚呈生物科技有限公司 | Method for removing resin substance from lignite wax |
| CN104370679B (en) * | 2014-10-17 | 2016-09-21 | 中国石油集团东北炼化工程有限公司吉林设计院 | The separating technology of removing butadiene dimer and device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257893A (en) * | 1998-12-19 | 2000-06-28 | 科莱恩有限公司 | Partial ester contg. polyol and montanin cerotic acid and wax preparation of montanin cerotic acid celcium soap |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257893A (en) * | 1998-12-19 | 2000-06-28 | 科莱恩有限公司 | Partial ester contg. polyol and montanin cerotic acid and wax preparation of montanin cerotic acid celcium soap |
Non-Patent Citations (2)
| Title |
|---|
| 王平 等.非苯溶剂提取褐煤蜡试验.《广西煤炭》.1994,第12卷(第2期),第85-88页. * |
| 郑筱梅 等.褐煤蜡精制方法研究.《重庆师范学院学报 自然科学版》.1988,第5卷(第2期),第55-58页. * |
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Owner name: GUODIAN FUEL LTD. Free format text: FORMER OWNER: CHINA UNIVERSITY OF MINING + TECHNOLOGY Effective date: 20130523 Owner name: CHINA UNIVERSITY OF MINING + TECHNOLOGY Effective date: 20130523 |
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Inventor after: Miao Yongqi Inventor after: Hu Guangzhou Inventor after: Cheng Gang Inventor after: Li Chunyan Inventor after: Ren Wei Inventor after: Zhang Shuangquan Inventor before: Hu Guangzhou Inventor before: Zhang Shuangquan |
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Free format text: CORRECT: INVENTOR; FROM: HU GUANGZHOU ZHANG SHUANGQUAN TO: MIAO YONGQI HU GUANGZHOU CHENG GANG LI CHUNYAN REN WEI ZHANG SHUANGQUAN Free format text: CORRECT: ADDRESS; FROM: 221116 XUZHOU, JIANGSU PROVINCE TO: 210031 NANJING, JIANGSU PROVINCE |
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Effective date of registration: 20130523 Address after: 210031 No. 10, Pudong Road, Nanjing, Jiangsu Patentee after: China Guodian Fuel Co., Ltd. Patentee after: China University of Mining & Technology Address before: 221116 Xuzhou Province,, China University of Mining and Technology, the southern loop of science and Technology Department of the three Patentee before: China University of Mining & Technology |
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