CN1803785A - Method for preparing furfural by utilizing cotton stalk - Google Patents
Method for preparing furfural by utilizing cotton stalk Download PDFInfo
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- CN1803785A CN1803785A CNA2006100422155A CN200610042215A CN1803785A CN 1803785 A CN1803785 A CN 1803785A CN A2006100422155 A CNA2006100422155 A CN A2006100422155A CN 200610042215 A CN200610042215 A CN 200610042215A CN 1803785 A CN1803785 A CN 1803785A
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- cotton stalk
- furfural
- hydrolysis
- acid
- pulverizing
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Abstract
The preparation method for furfural with cotton stalk comprises: cutting the cotton stalk into small bars of 2-5cm; further crushing and rolling to obtain the cotton stalk particles of 1-3cm as well as the corn core particle of 1-1.5cm; mixing the cotton stalk and corn core to stir with acid by great liquid and solid ratio in machine; then, loading into the hydrolysis kettle with filling density as 160-240kg/m3; leading vapor into the kettle, keeping the hydrolysis temperature as 145-180Deg for 2-5h as the hydrolysis period; leading the furfural primary liquid into post-process to extract, refine and obtain the final product. This invention improves yield, ensures product quality, and benefit to environmental protection.
Description
Technical field
The present invention relates to the preparation field of furfural, especially utilize cotton stalk to produce the method for furfural.
Background technology
Furfural is to fail synthetic with industrial chemicals so far and a kind of organic chemical industry's product that can only extract with plant materials such as agricultural wastes.Furfural is a kind of good selective solvent, also is the raw material of producing various furfuran compounds.It all has been widely used at aspects such as binder for casting, tetrahydrofuran (THF), lube oil finishing, organic synthesis, plastics, medicine, chemical anticorrosions.Furfural forms industrialized production in the world already, and producing and manufacturing technique has multiple, but all adopts direct method.Direct method is to put into a hydrolysis kettle containing the poly-pentose raw material, under the effect of catalyzer-sulfuric acid and heat, makes poly-pentose be hydrolyzed into pentose, the dehydrated again formation furfural of pentose simultaneously, then through extraction thick aldehyde, hair aldehyde continuous treating final the finished product furfural.The raw material of extraction furfural has a variety of, the higher raw material of all theoretically poly-pentose content, as: corn cob, sunflower seed shell, cotton stalk, cotton seed hulls, bagasse, rice husk, pourous wood etc. can extract furfural.But because hydrolysis stage exists special difficulty in process, make the raw material that uses in the suitability for industrialized production of present furfural mostly based on feed particulate material or the raw material easily pulverized, domestic mainly based on corn cob.And industrialized preparing process long for cotton stalk fiber, the assorted multiclass of a fork does not have stable practicality as yet like the agricultural crop straw raw material of wood structure.This situation makes that there is lack of raw materials becomes the important factor of restriction furfural production development.The hydrolysis process stage of extracting furfural mainly is divided into four procedures, promptly raw material pulverizing, with the mixing conveying, mix acid, hydrolysis of corn cob.With cotton stalk is that raw material extracts furfural in four procedures of hydrolysis stage, and the main technique difficulty of existence has 2 points.The one, the cutting of cotton stalk, pulverizing, because cotton stalk fiber is long, the branch fork is assorted many, can't directly pulverize, and with being shaft-like after the cutting of common chaffcutter and the stalk footpath is thick, quality is hard when mixing acid that diluted acid is difficult to penetrate in the plant structure, thereby make the mixed inhomogeneous hydrolysis of catalyzer incomplete, furfural dregs particle diameter after the hydrolysis is big, quality is hard, and acting as a fuel, it is not thorough to send into special-purpose seethe with excitement in the stove weak effect, burning of slag that easily cause when burning the slag boiler combustion.Thereby make the suitability for industrialized production that is used for furfural that cotton stalk can not be reliable and stable, limited the source of furfural raw material, the raising of restriction furfural output, also make agricultural waste material-cotton stalk can not the better synthesis utilization and agricultural waste material huddle to leave about and cause environmental pollution.The 2nd, the cotton stalk that crushes by 5～10% sour dense to mix the acid back pressure at water vapor in hydrolysis kettle be 0.45～0.75MPa, hydrolysis temperature is hydrolysis 2～5 hours under 145～180 ℃ the processing condition.In hydrolytic process,, the fluffy permeability of cotton stalk quality make the raw material hydrolysis incomplete because causing steam skewness in hydrolysis kettle to be prone to " gas passage " well; The hydrolysis end is arranged in the furfural dregs process and is easily caused " vapour hole " owing to the better depended on pressure deslagging of the fluffy ventilation property of cotton stalk quality, and row is unclean for slag, arranges continuously sometimes also can't drain several times only.And steam consumption is big especially, calculate the cost of the unit cost of steam consumption increase much larger than the cotton stalk low price reduction of raw material from cost, so comprehensive cost is uneconomic.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing cotton stalk to produce furfural, thus solve because of cotton stalk difficult broken can't mix acid and mix acid back dilute acid soln can't fully contact and use separately cotton stalk to cause deslagging difficulty, steam consumption height, a difficult problem that production cost is high with cotton stalk raw material.
Technical scheme of the present invention is: this kind utilizes cotton stalk to produce the method for furfural, comprise cotton stalk cut-out, pulverizing, conveying, batch mixing, mix acid, hydrolysis, distillation, it is characterized in that,
1), that whole cotton stalk is first through ZCQ4
ZH2Type rotor chaffcutter cuts into the cotton stalk rod of 2～5cm, and with three roller dusting machine dedustings, the cotton stalk rod further cuts, rubs the cotton stalk particle and the axially fragmentation of cotton stalk rod of cutting, pulverizing final one-tenth diameter 1～3cm through cutting, disintegrating apparatus again in cutting process; Be ground into the corn cob granule of 1～1.5cm after the dedusting of corn cob process vibratory screening apparatus with beater grinder;
2), the corn cob of cotton stalk after the pulverizing and usual method pulverizing is by specific mass ratio 0.5～1: 1 batch mixing, adopt bigger liquid solid to mix acid than the ratio of the quality of over dry raw material (quality of diluted acid and raw material moisture with), acid is dense to maintain 5～10%, pack into after mixing in acid mixer in the hydrolysis kettle, the packing density of mixing raw material is 160～240kg/m
3, feeding pressure in hydrolysis kettle is the water vapor of 0.45～0.75MPa, and keeping hydrolysis temperature is 145～180 ℃, and the hydrolysis cycle is 2～5 hours;
3), the furfural stoste that obtains in the hydrolytic process is introduced subsequent handling, after primary tower extracts hair aldehyde in furfural continuous treating equipment refining final commodity furfural.
Technique effect of the present invention is:
The present invention compared with prior art its characteristics, advantage and positively effect is mainly reflected in four aspects.
One has been to use the cutting of suitable cotton stalk raw material, the method and apparatus of pulverizing, makes production reliable and stable, can operate continuously move, and is suitable for suitability for industrialized production.Cotton stalk is difficult brokenly can't be mixed acid and mix the difficult problem that acid back dilute acid soln can't fully contact with cotton stalk raw material thereby solved, make cut-outs, the cotton stalk after pulverizing is thick by original stalk footpath, quality is hard, the crust fibers encapsulation closely, the wooden structures that is difficult for infiltrating dilute acid soln becomes the plant that particle is little, quality is fluffy, the herbaceous nature of dilute acid soln thoroughly, is easily infiltrated in the pulverizing of outer hide fiber.So more help the infiltration of dilute acid soln, make raw material and catalyst mix evenly shorten hydrolysis time, be more conducive to the comprehensive utilization of cotton stalk, improved the furfural productive rate.
The 2nd, preferably be suitable for the hydrolysis process condition of cotton stalk, enlarged furfural raw materials for production scope, reduced the furfural production cost, improved furfural yield, guaranteed the furfural quality.
The 3rd, cotton stalk low price mixes back unit raw materials cost with corn cob can descend nearly 20%, and the energy fecund is given birth to nearly 30% furfural dregs, the thermal value of cotton stalk slag and corn cob slag is similar substantially, can voluminous living nearly 1/3rd steam and electric power and about about 10～15% the coal of more piece but use the furfural dregs burning boiler to generate electricity simple the generating with corn cob slag burning boiler of ratio.Coal resources can fully utilize agricultural waste material, cleaner production under the intense situation day by day at home.The contribution that national economy has been done is huge.
The 4th, along with no longer acting as a fuel to burn but be deposited in the field, the cotton stalk of the raising of rural economy level rots, and not only pollute but also bring very big pressure to fire prevention at dry weather.The environmental issue that realization of the present invention can solve waste turns waste into wealth, and a kind of realistic approach is provided, and makes a large amount of agricultural crop straws be able to comprehensive utilization to obtain economic benefit.
Embodiment
Below provide two embodiment, the present invention is described in detail.
Embodiment 1:
Cotton stalk after raw material uses spring air-dry, its water-content is 22.5%.Cotton stalk is cut into the long segment of 4cm with chaffcutter earlier, in cutting process with three roller dusting machine dedustings.The cotton stalk rod that cuts is sent into cutting, disintegrating apparatus further cuts, the final one-tenth of pulverizing length is the cotton stalk particle about 1～1.5cm, be ground into the corn cob granule of 1～1.5cm after the dedusting of corn cob process vibratory screening apparatus with beater grinder, corn cob granule and cotton stalk particle are being pressed mass ratio 0.5～1 in the chapelet course of conveying: 1 thorough mixing, be transported to mix in the sour car by lift then and mix acid, catalyzer is a sulfuric acid, acid is dense 5～10%, remain on specific liquid solid than last with the acid amount, send in the hydrolysis kettle through rotary conveyor, the hydrolysis kettle volume is 10 cubic metres, adopt two still serial operations, the packing density of mixture is at 160～240kg/m
3, filling and feeding pressure behind the hydrolysis kettle is the water vapor of 0.45～0.75MPa, hydrolysis temperature is 145～180 ℃, hydrolysis 2 hours 45 minutes to 5 hours.The furfural stoste that hydrolysis obtains is introduced subsequent handling, and through extracting hair aldehyde, hair aldehyde continuous treating gets the commodity furfural.This routine furfural quality meets national top grade product standard, detects index and sees table 1 for details.This routine furfural yield is 7～8%, and every consumption sees table 2 for details.
Embodiment 2:
Corn cob after raw material uses spring air-dry, its water-content is 27%.Be ground into the corn cob granule of 1～1.5cm after the dedusting of corn cob process vibratory screening apparatus with beater grinder, be transported to mix in the sour car by lift then and mix acid, acid is dense 5～10%, remain on on the specific solid-to-liquid ratio with the acid amount, send in the hydrolysis kettle through rotary conveyor, the hydrolysis kettle volume is 10 cubic metres, adopts two still serial operations, and the packing density of corn cob is at 160～240kg/m
3, filling and feeding pressure behind the hydrolysis kettle is the water vapor of 0.45～0.75MPa, hydrolysis temperature is 145～180 ℃, hydrolysis 2 hours 45 minutes to 5 hours.The furfural stoste that hydrolysis obtains is introduced subsequent handling, and through extracting hair aldehyde, hair aldehyde continuous treating gets the commodity furfural.This routine furfural quality detecting index sees table 1 for details.This routine furfural yield is 8.5～9%, and every consumption sees table 2 for details.
Embodiment 3:
Used raw material, equipment and the operating process of this example is identical with embodiment 1.Processing condition are changed into: cotton stalk and corn cob were pressed mass ratio 0.4: 1.This routine furfural yield is 8～8.5%.Quality also reaches national top grade product index.The quality test index sees Table 1, and every consumption sees table 2 for details.
Table 1: embodiment furfural quality test result and GB 1926.1-88 set quota contrast table look-up
Table 2: embodiment furfural production cost contrast table
| The items of cost | Unit | The starting material unit price | Embodiment 1 | Embodiment 2 | Embodiment 3 | ||||
| Unit consumption | The amount of money | Unit consumption | The amount of money | Unit consumption | The amount of money | ||||
| Direct material | Corn cob | t | 400 | 7.05 | 2820 | 11.5 | 9.44 | 3776 | |
| Cotton stalk | t | 145 | 7.30 | 1058.5 | 3.78 | 548.1 | |||
| Sulfuric acid | kg | 623 | 618.8 | 620.6 | |||||
| Ground caustic | kg | 4.000 | 3.943 | 4.05 | |||||
| Power charge | The electricity charge | kW·h | 160.5 | 156.7 | 158.6 | ||||
| Steam | t | 26.5 | 27.6 | 27.1 | |||||
| Expense of raw materials adds up to | t | 3878.5 | 4600 | 4324.1 | |||||
Claims (1)
1, a kind of method of utilizing cotton stalk to produce furfural, comprise cotton stalk cut-out, pulverizing, conveying, batch mixing, mix acid, hydrolysis, distillation, it is characterized in that,
1), that whole cotton stalk is first through ZCQ4
ZH2Type rotor chaffcutter cuts into the cotton stalk rod of 2～5cm, and with three roller dusting machine dedustings, the cotton stalk rod further cuts, rubs the cotton stalk particle and the axially fragmentation of cotton stalk rod of cutting, pulverizing final one-tenth diameter 1～3cm through cutting, disintegrating apparatus again in cutting process; Be ground into the corn cob granule of 1～1.5cm after the dedusting of corn cob process vibratory screening apparatus with beater grinder;
2), the corn cob of cotton stalk after the pulverizing and usual method pulverizing is by specific mass ratio 0.5～1: 1 batch mixing, mix acid with certain liquid solid ratio, this liquid solid ratio makes acid densely maintain 5～10%, pack into after mixing in acid mixer in the hydrolysis kettle, the packing density of mixing raw material is 160～240kg/m
3, feeding pressure in hydrolysis kettle is the water vapor of 0.45～0.75MPa, and keeping hydrolysis temperature is 145～180 ℃, and the hydrolysis cycle is 2～5 hours;
3), the furfural stoste that obtains in the hydrolytic process is introduced subsequent handling, after primary tower extracts hair aldehyde in furfural continuous treating equipment refining final commodity furfural.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100422155A CN1803785A (en) | 2006-01-23 | 2006-01-23 | Method for preparing furfural by utilizing cotton stalk |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100422155A CN1803785A (en) | 2006-01-23 | 2006-01-23 | Method for preparing furfural by utilizing cotton stalk |
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| CN1803785A true CN1803785A (en) | 2006-07-19 |
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| CNA2006100422155A Pending CN1803785A (en) | 2006-01-23 | 2006-01-23 | Method for preparing furfural by utilizing cotton stalk |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659723A (en) * | 2012-04-27 | 2012-09-12 | 广州博能能源科技有限公司 | Process for preparing furfural by using agricultural by-products of high and crude fiber plants |
| CN103880792A (en) * | 2014-02-21 | 2014-06-25 | 魏新民 | Method for producing furfural through hydrolysis by using high-pressure two-kettle-cascade acid process |
| CN103898787A (en) * | 2012-12-25 | 2014-07-02 | 济南圣泉集团股份有限公司 | Comprehensive utilization method of biomass raw material |
| CN105777675A (en) * | 2016-05-09 | 2016-07-20 | 周家仁 | Method for preparing furfural by agriculture leftovers |
-
2006
- 2006-01-23 CN CNA2006100422155A patent/CN1803785A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659723A (en) * | 2012-04-27 | 2012-09-12 | 广州博能能源科技有限公司 | Process for preparing furfural by using agricultural by-products of high and crude fiber plants |
| CN102659723B (en) * | 2012-04-27 | 2016-02-03 | 北京博能康成科技有限公司 | The method of furfural is prepared with high robust fibre plant agricultural byproducts |
| CN103898787A (en) * | 2012-12-25 | 2014-07-02 | 济南圣泉集团股份有限公司 | Comprehensive utilization method of biomass raw material |
| CN103898787B (en) * | 2012-12-25 | 2016-06-15 | 济南圣泉集团股份有限公司 | A kind of comprehensive utilization process of biomass material |
| CN103880792A (en) * | 2014-02-21 | 2014-06-25 | 魏新民 | Method for producing furfural through hydrolysis by using high-pressure two-kettle-cascade acid process |
| CN105777675A (en) * | 2016-05-09 | 2016-07-20 | 周家仁 | Method for preparing furfural by agriculture leftovers |
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